HRID605143
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of N-(3-Bromo-phenyl)-4-chloro-3-nitro-benzamide (from Example 26A) (2.13 g, 6.0 mmol), 3-aminothiophenol (0.75 g, 6.0 mmol) and cesium carbonate (4.0 g, 12.0 mmol) in N,N-dimethylformamide (20 mL) was heated to 95° C. for 3 hours. After cooling to room temperature the mixture was poured into ice water (100 mL) and the resultant solution adjusted to pH 6 with 1N aqueous hydrochloric acid. The solution was then extracted with ethyl acetate (3×50 mL), the combined extracts dried over sodium sulfate, filtered and concentrated under vacuum to provide the title compound (2.87 g, 99%).
WORKUP
后处理
- extractionThe solution was then extracted with ethyl acetate (3×50 mL)
- dry with materialthe combined extracts dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated under vacuum