HRID1379376
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
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
- temperaturewas heated
- temperatureat reflux for 17 h
- temperatureAfter cooling
- concentrationconcentrated
- washwashed with water and brine
- dry with materialdried over MgSO4
- customevaporated to 23.59 g (92%) of an oil