HRID1740834

反应详情

EQUATION

反应方程式

HRID 1740834 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 7.85 g (0.0199 mole) of (Z)-2-[1-(4-chlorophenyl)-1-(4-methanesulphonylphenyl)methylene]succinic acid, prepared in example 28, in 40 ml of tetrahydrofuran are added dropwise 5.65 ml (0.0596 mole) of borane/dimethyl sulphide complex. The mixture is then stirred for 3 hours at ambient temperature and then 1 hour at 50° C. After returning to ambient temperature, 5 ml of ethanol are added dropwise. The mixture is then concentrated to half its volume and then taken up into water. The crystals obtained are filtered off under suction and washed with pentane and dried giving 6.92 g of (Z)-2-[1-(4-chlorophenyl)-1-(4-methanesulphonylphenyl)-methylene]-1,4-butanediol in the form of crystals with a melting point of 159-160° C.

WORKUP

后处理

  1. additionare added dropwise 5.65 ml (0.0596 mole) of borane/dimethyl sulphide complex
  2. custom1 hour
  3. customat 50° C
  4. customAfter returning to ambient temperature
  5. concentrationThe mixture is then concentrated to half its volume
  6. customThe crystals obtained
  7. filtrationare filtered off under suction
  8. washwashed with pentane
  9. customdried