HRID1756899

反应详情

EQUATION

反应方程式

HRID 1756899 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of KOH (4.21 g, 0.075 mol) in water (10 mL) was added to a solution of the 2-dodecyltetrazole acetic acid ethyl ester (23.2 g, 0.0715 mol) in ethanol (250 mL). The mixture was stirred at room temperature for 3 hours, concentrated in vacuo to ~50 mL, diluted with water (200 mL), and washed with ethyl acetate (100 mL). The aqueous layer was acidified with 1.0M HCl and extracted with ethyl acetate. The organic layer was dried over MgSO4, filtered, and concentrated to give 18.0 g, 85% of a white solid, mp 70°-73° C.

WORKUP

后处理

  1. concentrationconcentrated in vacuo to ~50 mL
  2. additiondiluted with water (200 mL)
  3. washwashed with ethyl acetate (100 mL)
  4. extractionextracted with ethyl acetate
  5. dry with materialThe organic layer was dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated