HRID1844771

反应详情

EQUATION

反应方程式

HRID 1844771 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a cold solution (5° C.) of 3.36 g of Intermediate 5, benzylamide in 40 mL of dichloromethane was added 6.02 mL of 36% HCl. The reaction mixture was stirred at room temperature until no starting material was observed by TLC. The organic phase was washed with 1N HCl (2×30 mL) and the combined aqueous phase basified to 10-12 with 25% NaOH. After saturating the aqueous phase with sodium chloride, it was extracted with dichloromethane (3×30 mL). The organic phase was dried and concentrated under vacuum yielding 2.01 g of a pale yellow oil.

WORKUP

后处理

  1. washThe organic phase was washed with 1N HCl (2×30 mL)
  2. concentrationAfter saturating the aqueous phase with sodium chloride, it
  3. extractionwas extracted with dichloromethane (3×30 mL)
  4. customThe organic phase was dried
  5. concentrationconcentrated under vacuum