天堂网亚洲,天天操天天搞,91视频高清,菠萝蜜视频在线观看入口,美女视频性感美女视频,95丝袜美女视频国产,超高清美女视频图片

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
010-86108875
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List BENZOIC ACID,4-BROMO-2-METHYL-,METHYL ESTER
99548-55-7

BENZOIC ACID,4-BROMO-2-METHYL-,METHYL ESTER synthesis

7synthesis methods
4-Bromo-2-methylbenzoic acid

68837-59-2

(TRIMETHYLSILYL)DIAZOMETHANE

18107-18-1

BENZOIC ACID,4-BROMO-2-METHYL-,METHYL ESTER

99548-55-7

Step 1: To a mixed solution of 4-bromo-2-methylbenzoic acid (15.1 g, 0.070 mol) in tetrahydrofuran (180 mL) and methanol (45 mL) was slowly added dropwise (trimethylsilyl) diazomethane in 2.0 M hexane solution (42 mL, 0.084 mol) at 0 °C. The reaction mixture was gradually warmed to room temperature and stirred continuously for 1 hour. Upon completion of the reaction, the solvent was removed by distillation under reduced pressure to afford methyl 4-bromo-2-methylbenzoate (16 g, 100% yield) as a yellow oil. The crude product could be used in the subsequent reaction without further purification. The product was characterized as follows: 1H NMR (400 MHz, CDCl3): δ 7.78 (d, 1H), 7.42 (s, 1H), 7.38 (d, 1H), 3.88 (s, 3H), 2.58 (s, 3H). Mass spectrum (EI): m/z 230 ([M+H]+, C9H9BrO2).

-

Yield:99548-55-7 100%

Reaction Conditions:

with sodium hydrogencarbonate in N,N-dimethyl-formamide at 80;

Steps:

5.5.76.1
5.76 l-(3-CHIX)RO-4-METHYI^PHENYLV3-r2-f2.6-DIOXO-PIPERrom- 3-YU-I-OXO-Z^-DIHYDRO-IH-ISOINDOL-S-YLMETHYLI-TJREA Step 1: A mechanically stirred mixture of 4-bromo-2-methyl-benzoic acid (100 g, 465 mmol), iodomethane (95 g, 670 mmol) and sodium bicarbonate (1 12 g, 1340 mmoi) in DMF (325 mL) was heated at 80 0C overnight. The reaction mixture was cooled to room temperature and partitioned between water (1500 mL) and 4: 1 hexanes:ethyl acetate (1500 mL). The organic layer was washed with water and dried (Na2SO4). The solvent was removed under vacuum to give HO g of 4-bromo-2-methyl-benzoic acid methyl ester as an oil, in 100% yield; 1H NMR δ 2.51 (s, 3H), 3.84 (s, 3H), 7.40-7.78 (m, 3H).

References:

CELGENE CORPORATION WO2008/27542, 2008, A2 Location in patent:Page/Page column 89-90

FullText

BENZOIC ACID,4-BROMO-2-METHYL-,METHYL ESTER Related Search: