HRID82708

反应详情

EQUATION

反应方程式

HRID 82708 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 3-(4-amino-1,2,5-oxadiazol-3-yl)-4-(3-chlorophenyl)-1,2,4-oxadiazol-5(4H)-one (30.0 mg, 0.107 mmol) and 4-dimethylaminopyridine (2.6 mg, 0.021 mmol) in pyridine (0.50 mL) was treated with benzeneacetyl chloride (42.6 μL, 0.322 mmol) and stirred for 4 h. The reaction mixture was concentrated and rediluted with ethanol (1.0 mL) and 2 M of sodium hydroxide in water (0.30 mL) stirred for 45 min. Purification of the crude reaction mixture by preparative HPLC gave the desired product (18 mg, 45%). LCMS for C17H15ClN5O3 (M+H)+: m/z=371.9.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. additionrediluted with ethanol (1.0 mL) and 2 M of sodium hydroxide in water (0.30 mL)
  3. stirringstirred for 45 min
  4. customPurification of the crude
  5. customreaction mixture by preparative HPLC