反应 #1876842

反应方程式

4-[(2-methylthio-ethyl)-(4-fluoro-benzoyl)-amino]-benzenesulfonamide

acetyl chloride

Et3N

→

4-[(2-methylthio-ethyl)-(4-fluoro-benzoyl)-amino]-N-acetyl-benzenesulfonamide

收率 81.0%

溶剂

CH2Cl2

反应条件

后处理

1. 1
   温度at reflux for 2 h
2. 2
   温度After cooling
3. 3
   其他the mixture was evaporated in vacuo
4. 4
   其他the residue was purified by MPLC (CH2Cl2 to 60:40 CH2Cl2/EtOAc)

实验过程

A solution of 4-[(2-methylthio-ethyl)-(4-fluoro-benzoyl)-amino]-benzenesulfonamide (0.32 g, 0.88 mmol), acetyl chloride (0.069 mL, 76 mg, 0.97 mmol), and Et3N (0.13 mL, 97 mg, 0.96 mmol) in CH2Cl2 (9 mL) was heated at reflux for 2 h. After cooling, the mixture was evaporated in vacuo, and the residue was purified by MPLC (CH2Cl2 to 60:40 CH2Cl2/EtOAc) to afford 0.29 g (81%) of 4-[(2-methylthio-ethyl)-(4-fluoro-benzoyl)-amino]-N-acetyl-benzenesulfonamide as a colorless glass; 1H NMR δ 2.03 (s, 3H), 2.15 (s, 3H), 2.77 (m, 2H), 4.15 (m, 2H), 6.90 (dd, 2H, J=7.5, 7.5), 7.24 (d, 2H, J=9.0), 7.32 (dd, 2H, J=3.0, 9.0), 7.92 (d, 2H, J=9.0), 9.1 (br s, 1H).

来源