HRID928414

反应详情

EQUATION

反应方程式

HRID 928414 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

A mixture of 1-(4-Hydroxymethyl-benzyl)-1H-[1,2,3]triazole-4-carboxylic acid ethyl ester (4.35 g, 9.42 mmol) and lithiumhydroxide-hydrate (1.976 g, 47.1 mmol) in 80 mL MeOH and 80 mL water was stirred at 30° C. for 3 h. The methanol was evaporated in vacuo. The residual aqueous layer was washed with ethyl acetate, acidified with 1 N aq. HCl and extracted with ethyl acetate. The organic layer was dried over MgSO4, filtered and evaporated to yield the crude product which was used in the next step without further purification. 1H-NMR (DMSO-d6, 400 MHz) 13.1 (broad s, 1H), 8.76 (s, 1H), 7.27-7.39 (m, 4H), 5.63 (s, 2H), 5.20 (t, 1H), 4.48 (d, 2H).

WORKUP

后处理

  1. customThe methanol was evaporated in vacuo
  2. washThe residual aqueous layer was washed with ethyl acetate
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic layer was dried over MgSO4
  5. filtrationfiltered
  6. customevaporated