HRID2265818

反应详情

EQUATION

反应方程式

HRID 2265818 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 4,4-bis(hydroxymethyl)-3,4-dihydro-2H-benzo[b]thiepin-5-one (424 mg, 1.78 mmol) in 22 ml of tetrahydrofuran were added, at 0° C., triethylamine (0.27 ml, 1.96 mmol) and cyclohexyl isocyanate (1.0 ml, 7.84 mmol). The mixture was stirred at 80° C. for 18 hours, concentrated and purified by column chromatography on silica (eluent: 1:2 tert-butyl methyl ether/cyclohexane). The product was obtained in a yield of 366 mg (57%).

WORKUP

后处理

  1. concentrationconcentrated
  2. custompurified by column chromatography on silica (eluent: 1:2 tert-butyl methyl ether/cyclohexane)
  3. customThe product was obtained in a yield of 366 mg (57%)