HRID275256

反应详情

EQUATION

反应方程式

HRID 275256 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a stirred suspension of 6.55 g (0.0584 mol) of potassium-t-butoxide in 60 mL dry dimethylformamide under nitrogen at 0° C. was added 6.84 mL (0.0584 mol) of benzyl mercaptan in 20 mL dimethylformamide while maintaining the temperature below 15° C. A solution of 15.83 g (0.053 mol) of the product from Example 2a or 2b in 20 mL dry dimethylformamide was added dropwise maintaining the temperature at 0° C. and then stirred another 30 minutes at 0° C. The reaction was poured into ice water and extracted with ether. The combined organic layers were washed with water, brine, dried over magnesium sulfate and evaporated to afford 17.84 g (100%). 1H NMR is similar to Example 3. IR (neat) 1725, 1675, 1575, 1135, 850 cm-1.

WORKUP

后处理

  1. temperaturewhile maintaining the temperature below 15° C
  2. extractionextracted with ether
  3. washThe combined organic layers were washed with water, brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. customto afford 17.84 g (100%)