HRID2265822

反应详情

EQUATION

反应方程式

HRID 2265822 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4,4-bis(hydroxymethyl)-3,4-dihydro-2H-benzo[b]thiepin-5-one (476 mg, 2.0 mmol) in 15 ml of tetrahydrofuran were added, at room temperature, triethylamine (0.31 ml, 2.2 mmol) and 1-naphthyl isothiocyanate (407 mg, 2.2 mmol). The mixture was heated to reflux for 24 hours, concentrated and purified by column chromatography on silica gel (eluent: 1:19 tert-butyl methyl ether/dichloromethane). The product was obtained in a yield of 87 mg (9%).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 24 hours
  3. concentrationconcentrated
  4. custompurified by column chromatography on silica gel (eluent: 1:19 tert-butyl methyl ether/dichloromethane)
  5. customThe product was obtained in a yield of 87 mg (9%)