反应详情

To a stirring solution of 4-bromo-2-chlorobenzoic acid (3.45 g, 15 mmol) and DIEA (7.7 ml, 44 mmol) in DMF (30 mL) was added HATU (6.1 g, 16 mmol) at 23° C. under nitrogen. Darkened suspension stirred for 1 h, then added n,o-dimethylhydroxylamine hydrochloride (2.1 g, 22 mmol). Solution stirred overnight at 23° C. Reaction then partitioned between 2.5% NaHCO3 (250 mL) and diethyl ether (100 mL). Aqueous further extracted with ether (2×50 mL). Combined ethereal extracts dried over MgSO4, then concentrated an amber oil under reduced pressure. 4-bromo-2-chloro-N-methoxy-N-methylbenzamide isolated as a light amber oil.

1. stirringSolution stirred overnight at 23° C
2. customReaction
3. customthen partitioned between 2.5% NaHCO3 (250 mL) and diethyl ether (100 mL)
4. extractionAqueous further extracted with ether (2×50 mL)
5. dry with materialdried over MgSO4
6. concentrationconcentrated an amber oil under reduced pressure