HRID2265827

反应详情

EQUATION

反应方程式

HRID 2265827 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 (720 mg, 3.02 mmol) in 38 ml of tetrahydrofuran were added, at room temperature, triethylamine (0.46 ml, 3.32 mmol) and 2,4-difluorophenyl isothiocyanate (985 μl, 7.55 mmol). The mixture was heated to reflux for 72 hours, concentrated and purified by column chromatography on silica gel (eluent: 1:2 ethyl acetate/hexane). The product was obtained in a yield of 170 mg (14%).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 72 hours
  3. concentrationconcentrated
  4. custompurified by column chromatography on silica gel (eluent: 1:2 ethyl acetate/hexane)
  5. customThe product was obtained in a yield of 170 mg (14%)