Tag: M.W=200-300

Adding a certain compound to certain chemical reactions, such as: 86845-27-4, name is 5-Bromo-2-methylbenzotrifluoride, 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 86845-27-4, Safety of 5-Bromo-2-methylbenzotrifluoride

A mixture of 4-methyl-3-trifluorobromobenzene (25 g, 104.59 mmol), N-bromosuccinimde (18.62 g, 104.59 mmol) and benzoyl peroxide (1.27 g, 5.23 mmol) in CCI4 (35 mL) was heated at 90 C for 4 hours. The reaction mixture was cooled to 0 C and then filtered through a glass frit washing with CH2CI2. The filtrate was concentrated and then purified by flash column chromatography (0% to 5% EtOAc in hexanes) to give the product as a clear oil that crystallized on standing (33.26 g, 100%). 1H NMR (400 MHz, CDCI3) 5 4.57 (s, 2H), 7.46 (d, J=8.3 Hz, 1 H), 7.67 (d, J=8.3 Hz, 1 H), 7.78 (s, 1H)

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-methylbenzotrifluoride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; PFIZER INC.; WO2006/18725; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 57946-63-1, These common heterocyclic compound, 57946-63-1, name is 2-Bromo-4-(trifluoromethyl)aniline, 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.

Diethyl ethoxymethylenemalonate (2.3 g, 10.6 mmol, 2.5 eq.) was added to a solution of 2-bromo-4-(trifluoromethyl)aniline (25) (1.0 g, 4.2 mmol, 1.0 eq.) in toluene (6 mL). The resulting mixture was refluxed for 11 h. After cooling to room temperature, the solvent was evaporated under reduced pressure. The residue obtained was purified by column chromatography (SiO2, cyclohexane/ethyl acetate, 100/0 to 80/20, v/v) to afford the desired product 26 (1.5 g, 3.7 mmol, 88percent) as a white solid. Rf (SiO2, cyclohexane/ethyl acetate, 9/1, v/v): 0.34; Mp: 90-92 °C; IR (cm-1): 1682 (nuC=O), 1646 (nuC=C), 1596 (deltaN-H), 1321 (nuCF3), 1245 (nuas C-O-C), 1077 (nus C-O-C); 1H NMR (CDCl3, 400 MHz) delta 11.38 (d, 1H, 3JNH-Ha= 12.7 Hz, NH), 8.48 (d, 1H, 3JHa-NH = 12.7 Hz, Ha), 7.86 (d, 1H, 4JH3-H5= 1.4 Hz, H3), 7.61 (m, 1H, H5), 7.36 (d, 1H, 3JH6-H5= 8.5 Hz, H6), 4.36 (q, 2H, 3JHd-He or Hd?-He?= 7.1 Hz, Hd or Hd?), 4.28 (q, 2H, 3JHd-He or Hd?-He?= 7.1 Hz, Hd or Hd?), 1.39 (t, 3H, 3JHe-Hd or He?-Hd?= 7.1 Hz, He or He?), 1.34 (t, 3H, 3JHe-Hd or He?-Hd?= 7.1 Hz, He or He?); 13C NMR (DMSO-d6, 125 MHz) delta 167.9 (Cc or Cc?), 164.8 (Cc or Cc?), 150.0 (Ca), 140.9 (C1), 130.5 (d, 3JC3-F = 4 Hz, C3), 126.6 (d, 3JC5-F = 4 Hz, C5), 125.6 (q, 2JC4-F = 33 Hz, C4), 123.7 (d, 1JCF3-F = 270 Hz, CF3), 117.2 (C2), 112.9 (C6), 97.5 (Cb), 60.7 (Cd or Cd?), 60.4 (Cd or Cd?), 14.6 (Ce or Ce?), 14.5 (Ce or Ce?); HRMS calculated for C15H1579BrF3NO4 [M+H]+ m/z 410.0215, found C15H1579BrF3NO4 [M+H]+ m/z 410.0189 (100percent); C15H1581BrF3NO4 [M+H]+ m/z 412.0157 (98percent).

The synthetic route of 57946-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Liu, Jianrong; Maisonial-Besset, Aurelie; Wenzel, Barbara; Canitrot, Damien; Baufond, Ariane; Chezal, Jean-Michel; Brust, Peter; Moreau, Emmanuel; European Journal of Medicinal Chemistry; vol. 136; (2017); p. 548 – 560;,
Bromide – Wikipedia,
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Related Products of 45762-41-2, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 45762-41-2, name is 4-Bromo-2-ethylaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of 4-bromo-2-ethylaniline (1.09g) in chloroform (20ml) was stirred at room temp. then treated with potassium acetate (0.49g) followed by acetic anhydride (0. 95ml). 18-Crown-6 (0.26g) and t-butylnitrite (1. 32ml) were added after 30 min and the mixture was stirred at reflux for 18h. The reaction mixture was diluted with chloroform and washed with saturated aqueous sodium hydrogen carbonate. The organic phase was separated using a hydrophobic frit and the solvent was evaporated to give the title compound as a brown solid (l. Og). NMR : 8H [CDC13] 8.30 (1H, d), 7.79 (1H, s), 7.63 (1H, d), 2.74 (3H, s), (2.55 (3H, s).

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-2-ethylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2004/10995; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 54962-75-3, name is 3-Bromo-5-(trifluoromethyl)aniline, A new synthetic method of this compound is introduced below., category: bromides-buliding-blocks

1,1-Cyclopropanedicarboxylic acid (2 g, 15.4 mmol) was dissolvedin anhydrous CH2Cl2, anhydrous triethylamine (2.2 mL) wasadded under nitrogen. The mixture was stirred on the ice-bath for30 min. Thionyl chloride (1.2 mL) in anhydrous CH2Cl2 was addeddropwise to the above mixture and stirring for 2 h. 5-bromo-3-(trifluoromethyl)-benzenamine (3.6 g, 15.4 mmol)dissolved inanhydrous CH2Cl2 was added into the mixture. Stirring wascontinued for 2 h and the solution was adjusted to pH 10 withNaOH (2 mol/L), after filtration and concentration in vacuo, anappropriate amount of water was added to the residues.The productwas extracted with ethyl acetate (50 mL), The organic layer wasseparated and the aqueous layer was adjusted to pH 2 with HCl(2 mol/L). The product was extracted with ethyl acetate (50 mL 3)again. The combined organic layer was concentrated in vacuo, totalyielding 1-[[(3,5-dimethylphenyl)amino]carbonyl] (9) (0.8 g, 37%).

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; Zhang, Lin; Shan, Yuanyuan; Li, Chuansheng; Sun, Ying; Su, Ping; Wang, Jinfeng; Li, Lisha; Pan, Xiaoyan; Zhang, Jie; European Journal of Medicinal Chemistry; vol. 127; (2017); p. 275 – 285;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 1435-51-4, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 1435-51-4 name is 1,3-Dibromo-5-fluorobenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

A mixture of Pd(OAc)2 (88 mg, 0.394 mmol) and BINAP (294 mg, 0.473 mmol) in dioxane (8 mL) was stirred in a sealed tube for ~5 min. To the mixture was then added l,3-dibromo-5-fluorobenzene (0.496 mL, 3.94 mmol) and (tetrahydro-2H-pyran- 4-yl)methanamine hydrochloride (299 mg, 1.969 mmol), stirring was continued for additional ~5 min and KOtBu (486 mg, 4.33 mmol) was added. The resulting mixture was heated at 93 C for ~18 hrs. The reaction mixture was cooled to room temperature, diluted with EtOAc (-50 mL) and MeOH (-10 mL), filtered off and concentrated under reduced pressure. The residue was purified by column chromatography [silica gel, 40 g, EtOAc/heptane = 5/95 to 30/70] providing 3-bromo-5-fluoro-N-((tetrahydro-2H-pyran- 4-yl)methyl)aniline (220 mg) as a colorless liquid. LCMS (m z): 289.9 [M+H]+; Rt = 1.03 min.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3-Dibromo-5-fluorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; NOVARTIS AG; PFISTER, Keith B; SENDZIK, Martin; WO2011/26917; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 13633-25-5, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 13633-25-5, name is 1-Bromo-4-phenylbutane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

17C Methyl 1-(4-phenylbutyl)-3-formylindole-5-carboxylate A solution of methyl 3-formylindole-5-carboxylate (2.234 g, 11.0 mmol) and potassium tert-butoxide (1.259 g, 11.2 mmol) in dry N,N-dimethylformamide (50 ml) was added with 1-bromo-4-phenylbutane (2.385 g, 11.2 mmol) and left under stirring at room temperature for 18 h. After that the solvent was evaporated off under reduced pressure, the resulting residue was partitioned between a NaCl saturated solution (50 ml) and chloroform (50 ml) and the aqueous phase was extracted with chloroform (3*50 ml). After drying and evaporating off the solvent under reduced pressure, a crude was obtained which was purified by chromatography through a silica gel column, eluding with n-hexane:ethyl acetate, 70:30, thereby obtaining 2.847 g of the title compound (87% yield). 1 H N.M.R. (300 MHz, CDCl3) delta ppm: 1.66 (m, 2H); 1.91 (m, 2H); 2.64 (t, 2H); 3.93 (s, 3H); 4.16 (t, 2H); 7.11 (d, 2H); 7.19 (m, 1H); 7.25 (d, 2H); 7.33 (d, 1H); 7.70 (s, 1H); 8.01 (dd, 1H); 8.99 (s, 1H); 9.98 (s, 1H).

The synthetic route of 1-Bromo-4-phenylbutane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Laboratorios Menarini S.A.; US5990142; (1999); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 2862-39-7, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 2862-39-7 as follows.

prepared as follows. Beta Alanine t-butyi ester, 10 nimoi, is dissolved in alcoholic sodium carbonate (O. I M), and 10 mmol of 2-NN ‘ dimethylamino ethyl bromide hydrobromide added thereto with stirring at room temperature, with the pH being monitored and maintained between 8.5 and 9.0 with the addition of aquous sodium hydroxide (1 M) as needed. Following cessation of base uptake, the reaction mixture is yophilized, and the product taken up in propanoi, free of inorganic salts.

According to the analysis of related databases, 2862-39-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; THROMBOLTYICS, LLC; CHIBBER, Bakshy, A.; (41 pag.)WO2016/73493; (2016); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 130723-13-6, name is 1-Bromo-3-fluoro-5-(trifluoromethyl)benzene, 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 130723-13-6, Application In Synthesis of 1-Bromo-3-fluoro-5-(trifluoromethyl)benzene

6-(3-Fluoro-5-trifluoromethylphenyl)-hex-5-ynoic Acid Methyl Ester (41). Pd(PPh3)2Cl2 (236 mg, 0.336 mmol) was added to a mixture of bromide 38 (1.677 g, 6.70 mmol) and methyl 5-hexynoate (1.025 g, 8.12 mmol) in triethylamine (5.0 mL) at room temperature. Cu(I)I (136 mg, 0.714 mmol) was added. The resulting mixture was stirred at room temperature for 1.5 h and at 80 C. for 22.5 h. The reaction mixture was cooled to room temperature, filtered through a short column of silica gel (5 g), and the column was washed with ethyl acetate. The organic solution was concentrated. The residue was purified by column chromatography on silica gel (40 g), eluting with EtOAc-hexanes (2%) to afford the product 41 (1.564 g) as a white solid in 81% yield: mp 44-45 C. IR (KBr) 3084, 2955, 2848, 2238, 1740, 1619, 1599, 1467, 1439, 1363, 1253, 1240, 1224, 1171, 1133, 1093, 1046, 995, 973, 924, 911, 875, 695 cm-1; 1H NMR (300 MHz, CDCl3) delta 7.40 (s, 1H), 7.21 (m, 2H), 3.66 (s, 3H), 2.47 (t, J=7.2 Hz, 4H), 1.90 (m, 2H); 13C NMR (75 MHz, CDCl3) delta 173.3, 163.7, 160.4, 132.8, 132.3, 126.8, 126.7, 124.7, 124.3, 121.8, 121.5, 112.3, 111.9, 79.1, 51.6, 32.7, 23.5, 18.7; ESIMS m/z (rel intensity) 288.96 (MH+, 51). Anal. (C14H12F4O2) C, H, F.

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, 1-Bromo-3-fluoro-5-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; PURDUE RESEARCH FOUNDATION; US2008/300288; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 626-40-4, name is 3,5-Dibromoaniline, A new synthetic method of this compound is introduced below., name: 3,5-Dibromoaniline

EXAMPLE 15 4,5-Dibromopyrrole-2-carboxylic acid (10 g., 0.037 mole) was converted to the corresponding acid chloride by reaction with 15 ml. of thionyl chloride, and the acid chloride dissolved in 25 ml. of benzene was reacted with 9.4 g. (0.037 mole) of 3,5-dibromoaniline in 50 ml. of pyridine using the procedure described above in Example 3. The product was recrystallized from an ethyl acetate/ethanol mixture to give 14.5 g. of 3′,4,5,5′-tetrabromopyrrole-2-carboxanilide, m.p. 244-245 C.

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:
Patent; Sterling Drug Inc.; US4046775; (1977); A;,
Bromide – Wikipedia,
bromide – Wiktionary

167355-41-1, name is 6-Bromo-1,2,3,4-tetrahydronaphthalen-2-amine, 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. Recommanded Product: 6-Bromo-1,2,3,4-tetrahydronaphthalen-2-amine

A solution of 6-bromo-1,2,3,4-tetrahydronaphthalen-2-amine (1.8 g, 7.96 mmol), benzyl chloroformate (1.6 g, 9.55 mmol), and Cs2CO3 (3 g, 21.71 mmol) in THF (20 mL) and water (20 mL) was stirred at 60 C overnight. After cooling to room temperature, the reaction mixture was extracted with EtOAc (30 mL x 3). The combined organic layer was dried over Na2SO4, filtered, and concentrated under vacuum. Purification by silica gel chromatography (eluting with gradient 1:100 to 1:3 EtOAc/pet. ether) afforded benzyl (6-bromo-1,2,3,4- tetrahydronaphthalen-2-yl)carbamate (Intermediate 8) as a solid. MS: (ESI, m/z): 360, 362 [M+H]t

The synthetic route of 167355-41-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FORMA THERAPEUTICS, INC.; ZABLOCKI, Mary-Margaret; GUERIN, David J.; NG, Pui Yee; WANG, Zhongguo; SHELEKHIN, Tatiana; CARAVELLA, Justin; LI, Hongbin; IOANNIDIS, Stephanos; (518 pag.)WO2019/32863; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary