HRID504587

反应详情

EQUATION

反应方程式

HRID 504587 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of racemic (2′S,3S,4′R)-6-chloro-4′-[5-chloro-2-(1-ethoxycarbonyl-1-propyl-butoxy)-phenyl]-2′-(5-chloro-2-methyl-phenyl)spiro[3H-indole-3,3′-piperidine]-2,6′(1H)-dione (280 mg, 0.41 mmol), LiOH.H2O (1 g, 24.6 mmol), H2O (12 mL) and methanol (38 mL) was refluxed for 2 h. After cooled to room temperature, the solution was concentrated and then the mixture was acidified to “pH” 1-2 by addition of concentrated HCl solution and then extracted with EtOAc. The combined organic layers were washed with water and brine, dried over anhydrous Na2SO4 and concentrated to give the title compound as a light yellow solid (220 mg).

WORKUP

后处理

  1. temperaturewas refluxed for 2 h
  2. concentrationthe solution was concentrated
  3. additionby addition of concentrated HCl solution
  4. extractionextracted with EtOAc
  5. washThe combined organic layers were washed with water and brine
  6. dry with materialdried over anhydrous Na2SO4
  7. concentrationconcentrated