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ChemicalBook CAS DataBase List tert-Butyl 2-bromo-5-methoxybenzoate
957063-12-6

tert-Butyl 2-bromo-5-methoxybenzoate synthesis

3synthesis methods
-

Yield:957063-12-6 90%

Reaction Conditions:

Stage #1: 2-bromo-5-methoxy-benzoic acidwith dmap;dicyclohexyl-carbodiimide in dichloromethane at 0; for 0.166667 h;
Stage #2: tert-butyl alcohol in dichloromethane at 20;

Steps:

Method B: General procedure for tBu protection

General procedure: To a solution of the acid (1 equiv.) in DCM (0.2 M) were added DCC (1.1 equiv.) and DMAP (0.5 equiv.) at 0 °C. After the mixture was stirred for 10 min, t-BuOH (1.5equiv.) was added. The reaction was stirred overnight at room temperature, then filtered through a pad of Celite and washed with Et2O three times. The combined organic layers were washed with brine, dried over Na2SO4 and concentrated. The crude product was purified by flash column chromatography on silica gel to give the desired product.

References:

Wang, Haifeng;Niu, Youhong;Zhang, Guoying;Ye, Xin-Shan [Tetrahedron Letters,2016,vol. 57,# 41,p. 4544 - 4548] Location in patent:supporting information

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