HRID2307549

反应详情

EQUATION

反应方程式

HRID 2307549 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dimethyl 4-(3-bromophenylsulphanylmethyl)phthalate (10 g, 26 mmol) is dissolved in 120 mL of anhydrous THF. 2.2 g of lithium borohydride (100 mmol) are then added slowly, after which the reaction medium is refluxed for 12 h. After cooling and treatment with saturated ammonium chloride solution, the reaction medium is extracted with ethyl acetate. The organic phases are combined, dried and concentrated under reduced pressure. The residue is purified by chromatography on a column of silica, to give a colourless oil (7.8 g, Y=89%).

WORKUP

后处理

  1. temperatureafter which the reaction medium is refluxed for 12 h
  2. temperatureAfter cooling
  3. extractiontreatment with saturated ammonium chloride solution, the reaction medium is extracted with ethyl acetate
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customThe residue is purified by chromatography on a column of silica
  7. customto give a colourless oil (7.8 g, Y=89%)