Tag: M.W=100-200

Synthetic Route of 59907-13-0, These common heterocyclic compound, 59907-13-0, name is 2-Bromo-1-fluoro-3-methylbenzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

2-bromo-3-fluorotoluene (1.89 g, 10 mmol),Carbazole (1.67 g, 10 mmol) and cesium carbonate (6.52 g, 20 mmol)Add 15mL dimethylformamide (DMF),The mixture was stirred at 150C for 12 hours, poured into 200 ml of water, and the precipitate was collected by filtration.After column purification, white solid 9-(2-bromo-3-methylphenyl)carbazole (3.1 g) was obtained with a yield of 92%.

The synthetic route of 59907-13-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chinese Academy Of Sciences Fujian Structure Of Matter Institute; Lu Canzhong; Chen Xulin; Jia Jihui; (22 pag.)CN107698613; (2018); A;,
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2695-48-9, name is 8-Bromo-1-octene, belongs to bromides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. name: 8-Bromo-1-octene

THF (21 mL) was coolecd to -50 C, n-BuLi (2.5 M, 10.3 mL) was added dropwise. After addition, i-Pr2 H (2.6 g, 25.7 mmol, 3.6 mL) was added to the solution dropwise. After addition, the solution was stirred at -50 C for 0.5 hr. Then the solution was warmed up to -30 C, and a solution of compound 14A (1.4 g, 10.3 mmol, 1.4 mL) in THF (10 mL) and Heptane (10 mL) was added. Then a solution of compound 14B (2.4 g, 12.4 mmol, 2.1 mL) in THF (8 mL) was added. The reaction was stirred at -30 C for lhr. The mixture was quenched with H20 (100 mL). The organics were separated and extracted with H20 (50 mL x 2). The aqueous phase was acidified with IN HCl to pH ~ 2 and then extracted with EtOAc (100 mL x 2). The organics were collected, dried with Na2S04, filtered and concentrated to afford compound 14C (4.4 g, crude) as light yellow oil, which was used directly for the next step without further purification. 1H NMR (CDCI3, 400 MHz): delta 7.90 – 7.88 (m, 1H), 7.34 – 7.31 (m, 1H), 7.15 – 7.09 (m, 2H), 5.72 – 5.63 (m, 1H), 4.87 – 4.76 (m, 2H), 2.90 – 2.86 (m, 2H), 1.92 – 1.87 (m, 2H), 1.50 – 1.47 (m, 2H), 1.26 – 1.14 (m, 8H).

The synthetic route of 2695-48-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BLADE THERAPEUTICS, INC.; BUCKMAN, Brad, Owen; YUAN, Shendong; MA, Jingyuan; EMAYAN, Kumaraswamy; ADLER, Marc; (327 pag.)WO2018/9417; (2018); A1;,
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Adding a certain compound to certain chemical reactions, such as: 6911-87-1, name is 4-Bromo-N-methylaniline, belongs to bromides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 6911-87-1, Recommanded Product: 6911-87-1

2 mmol of trifluoroethylamine hydrochloride, 1 mL of water, 34 uL of acetic acid, and 1 mL of dichloroethane were placed in a reaction tube, and a rubber stopper was placed and fixed on a stirrer. Take 42 mg of sodium nitrite in a 1.5 mL sample tube, add 1 mL of water to the sample tube, and shake the sample.The tube is dissolved in sodium nitrite. dissolving the dissolved sodium nitrite solution into the reaction tube with a syringe, Stir for half an hour at room temperature.Dissolve the iron porphyrin of formula 3 with 1 mL of dichloromethane (R1 = calixarene, R2 = R3 = CN, L = OAc)(catalytic amount, 9/1000 of the molar amount of secondary amine), 0.24 mmol of 4-bromo-N-methylaniline was taken in the sample tube. After half an hour, put the sample tube the internal mixed solution is added dropwise to the reaction tube, and stirred while being added.The temperature was raised to 80 C for 12 hours. The reaction solution is cooled to room temperature and passedPart of the impurities are removed by filtration, concentrated and purified by column chromatography to obtain the desired product. The column chromatography eluent is petroleum ether andA mixed solvent of acetone. The structure of 4-bromo-N-methyl-N-(2,2,2-trifluoroethyl)aniline is as follows:The compound was a pale yellow liquid with a yield of 73% and its nuclear magnetic data was as follows:

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 4-Bromo-N-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Yuanjiang Hualong Catalysis Technology Co., Ltd.; Liu Qiang; Xu Guiming; Guo Cancheng; (16 pag.)CN108997145; (2018); A;,
Bromide – Wikipedia,
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Reference of 4333-56-6, A common heterocyclic compound, 4333-56-6, name is Bromocyclopropane, molecular formula is C3H5Br, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

In a microwave reaction vial, 4-hydroxybenzaldehyde (1.20 g), K2CO3 (2.04 g), and NaI(49.0 mg), bromocyclopropane (1.02 mL), and DMF (9.80 mL) were mixed and the vialwas sealed. The mixture was stirred for 3 h at 200 oC with microwave irradiation. Aftercooled to room temperature, the mixture was poured into water and extracted with Et2O3 times. Combined organic layers were washed with brine, passed through PhaseSeparator, and concentrated under reduced pressure. The residue was purified by flashcolumn chromatography (gradient from hexane to hexane/EtOAc = 1:1) to give 3h (510mg) as a colorless oil. 1H NMR (300 MHz, CHLOROFORM-d) delta ppm 0.76 – 0.91 (m, 4 H) 3.77 – 3.88 (m, 1 H) 7.12 – 7.19 (m, 2 H) 7.80 – 7.87 (m, 2 H) 9.90 (s, 1 H).MS ESI/APCI Dual posi: 163[M+H]+, 185[M+Na]+.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Article; Hamada, Makoto; Takayama, Tetsuo; Shibata, Tsuyoshi; Hiratate, Akira; Takahashi, Masato; Yashiro, Miyoko; Takayama, Noriko; Okumura-Kitajima, Lisa; Koretsune, Hiroko; Kajiyama, Hiromitsu; Naruse, Takumi; Kato, Sota; Takano, Hiroki; Kakinuma, Hiroyuki; Bioorganic and Medicinal Chemistry Letters; vol. 28; 10; (2018); p. 1725 – 1730;,
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Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 586-61-8, name is 1-Bromo-4-isopropylbenzene, A new synthetic method of this compound is introduced below., Safety of 1-Bromo-4-isopropylbenzene

Under a stream of nitrogen, 2.55 g (105 mmol) of magnesium and 50 ml of anhydrous THF were put into a nitrogen-replaced 300 ml capacity reaction flask, followed by stirring. At room temperature, a 30 ml THF solution of 19.91 g (100 mmol) of 4-t-propylphenylbromobenzene was added dropwise thereto, followed by stirring at room temperature for 1 hour (synthesis of a Grignard compound).Next, the above-mentioned solution was cooled to 5 C. or less, and 10.05 g (50 mmol) of the (S)-proline-N-ethyl carbamate methyl ester obtained in Synthesis Example 2 was added dropwise thereto at 10 C. or less and allowed to undergo the reaction. Thereafter, this was heated under reflux for 3 hours and then cooled, and the reaction solution was added to 100 ml of saturated ammonium chloride aqueous solution, mixed with 100 ml of toluene for extraction, followed by stirring for 1 hour. This was transferred to a separating funnel, and the organic layer was separated and washed twice with saturated brine. After drying the organic layer with anhydrous sodium sulfate, the solvent was evaporated to obtain 16.22 g of (5S)-[3,3,0]-1-aza-2-oxo-3-oxa-4,4-bis-(4′-i-propylphenyl)-bicyclooctane.

The synthetic route of 586-61-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TAKASAGO INTERNATIONAL CORPORATION; US2010/324338; (2010); A1;,
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Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 348-57-2, name is 1-Bromo-2,4-difluorobenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 1-Bromo-2,4-difluorobenzene

To a solution of compound 97-4 (10 g, 51 mmol) in anhydrous THF (100 mL) was added slowly LDA (25 mL, 62 mmol) at ?78¡ã C., and the reaction solution was stirred for 1 h, after which ethylchlorosilane (10.5 mL, 57 mmol) was added and the resulting solution was stirred ?78¡ã C. for 2 h. After TLC indicated the reaction was complete, the reaction was quenched with saturated NH4Cl solution (aq., 100 mL), and the aqueous phase was extracted with EtOAc (200 mL¡Á3). The organic phases were combined, dried over anhydrous Na2SO4, filtered and evaporated to dryness by rotatory evaporation to give compound 97-5 (15.7 g, Yield 100percent, colourless oily liquid) which was directly used for the next step. LCMS (ESI) m/z: 309 (M+1) 1H NMR (CDCl3, 400 MHz): delta ppm 7.53-7.47 (m, 1H), 6.74 (t, J=8.4 Hz, 1H), 0.98-0.82 (m, 15H)

The synthetic route of 348-57-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hubei Bio-Pharmaceutical Industrial Technological Institute Inc.; Humanwell Healthcare (Group) Co., Ltd.; Wang, Xuehai; Wu, Chengde; Xu, Yong; Shen, Chunli; Li, Li’e; Hu, Guoping; Yue, Yang; Li, Jian; Guo, Diliang; Shi, Nengyang; Huang, Lu; Chen, Shuhui; Tu, Ronghua; Yang, Zhongwen; Zhang, Xuwen; Xiao, Qiang; Tian, Hua; Yu, Yanping; Chen, Hailiang; Sun, Wenjie; He, Zhenyu; Shen, Jie; Yang, Jing; Tang, Jing; Zhou, Wen; Yu, Jing; Zhang, Yi; Liu, Quan; (251 pag.)US2017/313683; (2017); A1;,
Bromide – Wikipedia,
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Related Products of 4333-56-6,Some common heterocyclic compound, 4333-56-6, name is Bromocyclopropane, molecular formula is C3H5Br, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

A mixture of 5-bromo-2-chlorophenol (543 mg, 2.62 mmol), bromocyclopropane (836 mul, 10.47 mmol) and caesium carbonate (1.701 g, 5.24 mmol) in N,N-dimethylacetamide (7.5 ml) was stirred for 47 h at 150 C. After 25.25 h further bromocyclopropane (836 mul, 10.47 mmol) was added. The reaction mixture was poured onto ice-water (40 ml) and set to pH=2 with aqueous HCl (1 N, 9.5 ml). This mixture was extracted with TBME (twice 50 ml). The organic layers were washed with brine (40 ml), combined and dried over sodium sulfate. Concentration and purification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 67:33) afforded the title compound (570 mg, 87%) as a light yellow oil. MS m/e: 248.0 [M+H]+

The synthetic route of 4333-56-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Knust, Henner; Nettekoven, Matthias; Pinard, Emmanuel; Roche, Olivier; Rogers-Evans, Mark; US2009/312314; (2009); A1;,
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Adding a certain compound to certain chemical reactions, such as: 2270-59-9, name is 5-Bromo-2-methylpent-2-ene, belongs to bromides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 2270-59-9, Safety of 5-Bromo-2-methylpent-2-ene

Potassium carbonate (49 mg), potassium iodide (29.4 mg) and 5-bromo-2-methyl- 2-pentene (35.3 muL) was added to a solution of Compound No. 12 (62 mg) in acetonitrile (3 mL). The mixture was stirred at 800C for 5 hours and subsequently at room temperature overnight. The mixture was concentrated under reduced pressure and the residue thus obtained was partitioned between dichloromethane and water. The separated organic layer was washed with water and brine, dried over anhydrous sodium sulphate and concentrated under reduced pressure. The residue thus obtained was purified by preparative column chromatography to yield the title compound. Yield: 27mg1H NMR (CDCl3):delta 7.43-7.33 (1OH, m), 5.07-5.04 (IH, m), 3.65-3.47 (IH, m), 3.15-2.05 (13H, m), 21.78-1.73 (6H, m), 1.33-1.1 (4H, m).Mass (m/z): 433 (M++.).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 5-Bromo-2-methylpent-2-ene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; RANBAXY LABORATORIES LIMITED; WO2007/39884; (2007); A1;,
Bromide – Wikipedia,
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Related Products of 1422-54-4,Some common heterocyclic compound, 1422-54-4, name is 2-Bromo-6-fluorotoluene, molecular formula is C7H6BrF, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

1-Bromo-3-fluoro-2-methylbenzene (388 mg, 2.05 mmol), and (4-methoxyphenyl)methanol (0.511 mL, 4 mmol) were dissolved in DMF (5 mL) in a microwave vessel. Sodium hydride as a 60% dispersion in mineral oil (164 mg, 4.0 mmol) was added portionwise under a flow of nitrogen over 10 min. The reaction vessel was then sealed and heated at 180 C. for 900s. The crude reaction mixture was poured onto 1:1 water:brine (6 mL) and DCM (10 mL). The biphasic mixture was stirred at ambient temperature for 1 h and then the organic and aqueous layers were separated. The combined organics were dried over Na2SO4 and concentrated in vacuo. The crude material was then purified by chromatography on silica gel. Elution with 5:95 ethyl acetate:heptane afforded 1-bromo-3-(4-methoxybenzyloxy)-2-methylbenzene (289 mg, 0.9 mmol, 46%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Bromo-6-fluorotoluene, its application will become more common.

Reference:
Patent; N.V. Organon; US2007/185156; (2007); A1;,
Bromide – Wikipedia,
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Application of 3814-30-0, These common heterocyclic compound, 3814-30-0, name is (Bromomethyl)cyclopentane, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: To a solution of 6 (0.16 g, 0.85 mmol) in DMF (10 mL) was added K2CO3 (0.19 g, 1.40 mmol) and a solution of R1Br (1.0 mmol) in DMF (3 mL) was added dropwise. The reaction mixture was warmed to 70C and stirred for 6-12 h. After cooling to room temperature, the mixture was then poured in water (80 mL) and extracted with EtOAc (3 ¡Á 20 mL), and then washed with brine, dried with Na2SO4. The organic extracts were concentrated in vacuo and the residue was purified by flash chromatography (dichloromethane/methanol) to yield target compounds A1-A14 in yields ranging from 68.7% to 77.3%.

Statistics shows that (Bromomethyl)cyclopentane is playing an increasingly important role. we look forward to future research findings about 3814-30-0.

Reference:
Article; Wang, Yinhu; Mowla, Rumana; Guo, Liwei; Ogunniyi, Abiodun D.; Rahman, Taufiq; De Barros Lopes, Miguel A.; Ma, Shutao; Venter, Henrietta; Bioorganic and Medicinal Chemistry Letters; vol. 27; 4; (2017); p. 733 – 739;,
Bromide – Wikipedia,
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