HRID847618

反应详情

EQUATION

反应方程式

HRID 847618 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To sodium (3.05 g, 133 mmol) in methanol (135 ml) was added tert-butylmercaptan (17.0 ml, 151 mmol). After 20 min methyl a-benzylacrylate (17.05 g, 96.8 mmol) in methanol (100 ml) was added and after 1 h at room temperature the mixture was heated at reflux for 17 h. After cooling, the mixture was acidified with 2M HCl (70 ml), concentrated, taken up in ether, washed with water and brine, then dried over MgSO4 and evaporated to 23.59 g (92%) of an oil. 1H NMR (CDCl3) δ 7.15-7.35 (m,5H), 3.63 (s,3H), 2.60-3.05 (m,5H), 1.28 (s,9H).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 17 h
  3. temperatureAfter cooling
  4. concentrationconcentrated
  5. washwashed with water and brine
  6. dry with materialdried over MgSO4
  7. customevaporated to 23.59 g (92%) of an oil