HRID40554

反应详情

EQUATION

反应方程式

HRID 40554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.43 g of tert-butyl ester of 4-[5-(4-methyl-4-phenyl-[1,4]azasilinan-1-yl)-pyridin-2-yl]-3,4-dihydro-2H-quinoxaline-1-carboxylic acid is put in 50 mL of dichloromethane and after cooling on an ice bath, 3.5 mL of a 4N solution of hydrochloric acid in dioxane is added. The reaction mixture is stirred for 16 h. After concentration, the mixture is taken up in dichloromethane, and neutralized by adding a saturated solution of sodium bicarbonate. After decanting, the aqueous phase is extracted with dichloromethane. The dichloromethane phases are combined and dried over sodium sulfate. After concentration under vacuum, 0.338 g of 1-[5-(4-methyl-4-phenyl[1,4]azasilinan-1-yl)-pyridin-2-yl]-1,2,3,4-tetrahydroquinoxaline is obtained.

WORKUP

后处理

  1. temperatureafter cooling on an ice bath
  2. concentrationAfter concentration
  3. additionby adding a saturated solution of sodium bicarbonate
  4. customAfter decanting
  5. extractionthe aqueous phase is extracted with dichloromethane
  6. dry with materialdried over sodium sulfate
  7. concentrationAfter concentration under vacuum