HRID1297483

反应详情

EQUATION

反应方程式

HRID 1297483 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

S-t-butyl Thiobenzoate t-Butyl Mercaptan (6.15 g, 0.068 mol) was added dropwise to a solution of benzoyl chloride (10.5 g, 0.075 mol) in pyridine (6 g). The resulting mixture was allowed to stir for two hours at room temperature then poured onto ice-water and the mixture extracted with diethyl ether. The organic extract was washed with dilute HCl, water and brine and finally dried over anhydrous sodium sulfate. After removal of solvent and vacuum distillation, S-t-butyl thiobenzoate was obtained (6.64 g, 50.1% yield), b.p. 86° C. (0.8 mmHg). 1H-nmr (CDCl3) d (ppm): 1.60 (s, 9H, 3×CH3), 7.41 (m, 2H, ArH), 7.54 (m, 1H, ArH) and 7.94 (d, 2H, ArH). 13C-nmr (CDCl3) d (ppm): 29.8, 48.0, 126.8, 128.3, 132.7, 138.6 and 192.9. ii) t-Butyl Dithiobenzoate

WORKUP

后处理

  1. additionthen poured onto ice-water
  2. extractionthe mixture extracted with diethyl ether
  3. extractionThe organic extract
  4. washwas washed with dilute HCl, water and brine
  5. dry with materialfinally dried over anhydrous sodium sulfate
  6. customAfter removal of solvent and vacuum distillation