HRID2049331

反应详情

EQUATION

反应方程式

HRID 2049331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-(3-hydroxyphenyl)hexahydro-2H-azepin-2-one (2.05 g) in dry DMF was added dropwise to a suspension of sodium hydride (0.3 g). After 30 minutes at ambient temperature, benzyl chloride (1.3 g) was added. The mixture was stirred for a further 2 hours and then cooled, and treated with water. The resulting solution was extracted several times with toluene, and the combined toluene layers washed thoroughly with water. The solvent was evaporated to give an oil that crystallised from ethyl acetate to give the title compound as a white solid (1.4 g) m.p. 119°-122° C.

WORKUP

后处理

  1. temperaturecooled
  2. extractionThe resulting solution was extracted several times with toluene
  3. washthe combined toluene layers washed thoroughly with water
  4. customThe solvent was evaporated
  5. customto give an oil that
  6. customcrystallised from ethyl acetate