HRID748761

反应详情

EQUATION

反应方程式

HRID 748761 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Process 1: At 0° C., lithium aluminum hydride (a 1.0M tetrahydrofuran solution, 6.74 ml, 6.74 mmol) was added dropwise to a tetrahydrofuran solution (10 ml) of the ethyl 3-[(4-chlorophenyl)sulfonyl]-3-(2,5-difluorophenyl)propionate (1.31 g, 3.37 mmol) obtained in Example 25. The mixture was then was stirred at room temperature for 3 hours. After cooling the reaction mixture to 0° C., and addition of a saturated aqueous ammonium chloride solution, the mixture was stirred at room temperature for 15 hours. The solid thus precipitated was filtered off. The solution thus obtained was diluted with ether, washed with brine, dried over magnesium sulfate and then, concentrated. The residue thus obtained was recrystallized from ethyl acetate-hexane, whereby the title compound (397 mg, 1.14 mmol, 34%) was obtained as a colorless solid.

WORKUP

后处理

  1. temperatureAfter cooling the reaction mixture to 0° C.
  2. stirringthe mixture was stirred at room temperature for 15 hours
  3. customThe solid thus precipitated
  4. filtrationwas filtered off
  5. customThe solution thus obtained
  6. washwashed with brine
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated
  9. customThe residue thus obtained