HRID2265824

反应详情

EQUATION

反应方程式

HRID 2265824 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]oxepin-5-one (500 mg, 2.25 mmol) in 28 ml of tetrahydrofuran were added, at room temperature, triethylamine (0.34 ml, 2.5 mmol) and phenyl isothiocyanate (672 μl, 5.63 mmol). The mixture was heated to reflux for 72 hours, concentrated and purified by column chromatography on silica gel (eluent: 1:1 tert-butyl methyl ether/cyclohexane). The product was obtained in a yield of 149 mg (19%).

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: 1:1 tert-butyl methyl ether/cyclohexane)
  5. customThe product was obtained in a yield of 149 mg (19%)