HRID1470308

反应详情

EQUATION

反应方程式

HRID 1470308 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl 4-(benzyloxy)-2-(1H-pyrazol-1-yl)pyrimidine-5-carboxylate, 3-b, (150 g, 0.46 mol) in THF (1.5 L) was treated with LiOH monohydrate (58 g, 1.39 mol) in water (60 ml) at room temperature for 3 hours. The mixture was concentrated under vacuum and diluted with water (200 ml) followed by extraction with ethyl acetate. The aqueous layer was acidified to pH=2 with 10% HCl and solid crushed out from the solution which was then filtered and washed with water to afford the compound, 3-c. (40 g, 29%).

WORKUP

后处理

  1. concentrationThe mixture was concentrated under vacuum
  2. additiondiluted with water (200 ml)
  3. extractionfollowed by extraction with ethyl acetate
  4. customcrushed out from the solution which
  5. filtrationwas then filtered
  6. washwashed with water