Category: 6698-13-1

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. 6698-13-1, name is 4-Bromo-1,3-benzodioxole, A new synthetic method of this compound is introduced below., Safety of 4-Bromo-1,3-benzodioxole

[0907] Method 3: To a stirred mixture of 5-(4-fluorophenyl)-4-methylpyridin-2(1H)-one (2.04 g, 10 mmol, 1.0 eq.), 4-bromobenzo[d][1,3]dioxole (3.0 g, 15 mmol, 1.5 eq.), and K2C03 (2.76 g, 20 mmol, 2eq.) in DMF (50 mL) was added CuT (191 mg, 1 mmol, 0.1 eq.) and 8- hydroxyquinoline (140 mg, 1 mmol, 0.1 eq.). The reaction mixture was stuffed at 140C for 3 days under N2 protection. The mixture was cooled to rt, diluted with EA (250 mL), washed with water and brine, concentrated. The residue was purified by flash chromatography on silica gel (PE:EA=5:1-*1:1) to yield Compound 184 (680 mg, 21% yield) as white solid. ?H NMR (CDC13, 400 MHz) (57.35-7.32 (m, 2H), 7.26 (s, 1H), 7.18 (t, J=8.8Hz, 2H), 7.02-6.94 (m, 3H), 6.67 (s, 1H),6.13 (s, 2H), 2.21 (s, 3H). MS (ES) m/z [M+Hf? 323.8.

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; INTERMUNE, INC.; RAMPHAL, Johnnie, Y.; BUCKMAN, Brad, Owen; EMAYAN, Kumaraswamy; NICHOLAS, John, Beamond; SEIWERT, Scott, D.; WO2015/153683; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 6698-13-1, 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. 6698-13-1, name is 4-Bromo-1,3-benzodioxole belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

nBuLi (2.5M in hexanes, 2.38 mL, 5.97 mmol) was dropwise added to a solution of 4- bromo-1 ,3-benzodioxole (1 g, 4.97 mmol) and triisopropyl borate (1.49 mL, 6.47 mmol) in 50 mL of dry tetrahydrofuran at -78 0C under argon. The reaction was maintained at that temperature for 3 hours, then warmed up to room temperature and cooled back to 0 0C immediately. The solution was acidified to pH=2 with HCI 2N and neutralized to pH=7 with NaOH 2N, it was then extracted with ethyl acetate (3 x 25 ml), the organic solution was washed with brine, dried over sodium sulphate and the solvent removed under reduced pressure to yield the title compound (570 mg, 69%) as a white solid. H1-NMR delta (CD3OD): 5.92 (s, 2H), 6.80-6.86 (m, 3H).

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-1,3-benzodioxole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; LABORATORIOS ALMIRALL, S.A.; WO2007/96072; (2007); A2;,
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. 6698-13-1, name is 4-Bromo-1,3-benzodioxole, A new synthetic method of this compound is introduced below., Quality Control of 4-Bromo-1,3-benzodioxole

The compound 4-bromobenzo[d][1,3]dioxole (5g, 24.873mmol)And sublimation sulfur (0.848g, 26.2mmol) was added to the two-necked flask, under the protection of nitrogen, was added tetrahydrofuran (100mL), cooled to -70 and stirred for 30 minutes,Slowly add hexane solution of tert-butyllithium (38mL, 49mmol, 1.3mol/L),After the dropwise addition, the reaction was continued at this temperature for 2 hours,Saturated ammonium chloride solution (100 mL) was added dropwise to quench the reaction, ethyl acetate (200 mL) was added for extraction, liquid separation, the organic phase was washed with 2N sodium hydroxide solution (20 mL), and the aqueous phases were combined,After adjusting the pH of the aqueous phase to about 4-5 with 4N hydrochloric acid, extract the aqueous phase with ethyl acetate (100 mL×2),The organic phases were combined, and the organic phase was washed with saturated sodium chloride solution (100 mL), dried over anhydrous sodium sulfate, and filtered.The filtrate was concentrated under reduced pressure to give the title compound as a yellow oil (3.12g, 81.4%).

The synthetic route of 6698-13-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Luo Huichao; Ren Qingyun; Yin Junjun; Wu Chunlin; Fan Yuxin; Mo Yufeng; Zhang Yingjun; (102 pag.)CN111057074; (2020); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 6698-13-1, name is 4-Bromo-1,3-benzodioxole, molecular formula is C7H5BrO2, 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. HPLC of Formula: C7H5BrO2

General procedure: An oven dried pressure tube was charged with aryl halide (0.5mmol), CuI (10-25mol%), anhydrous Zn(OAc)2 (1.5-2equiv) and anhydrous DMSO (1.6mL). The tube was sealed with a Teflon screw cap and stirred at 135C for 24-36h. The reaction mixture was then cooled to room temperature and stirred in 10mL of diethyl ether for 5min. It is filtered through a sintered funnel and the filtrate is washed with excess ice cold water and further extracted with diethyl ether (3¡Á10mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to give the crude product, which was purified by column chromatography using 200-400 mesh silica gel and a mixture of diethyl ether and hexane (or pentane, for Table 2, entries 2, 8, 10, 14, 16 and 24) as eluents to afford the desired products in good yields.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 6698-13-1, its application will become more common.

Reference:
Article; Joseph, P.J. Amal; Priyadarshini; Kantam, M. Lakshmi; Sreedhar; Tetrahedron; vol. 69; 38; (2013); p. 8276 – 8283;,
Bromide – Wikipedia,
bromide – Wiktionary