HRID1889110

反应详情

EQUATION

反应方程式

HRID 1889110 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 3-(1,2,4-thiadiazol-5-yl)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyrazine (I115) (50 mg, 0.240 mmol) and triethylamine (0.050 mL, 0.360 mmol) in DCM (1.5 ml) was treated with 3-chloro-4-fluoro-2-methylbenzoyl chloride (I58) (54.7 mg, 0.264 mmol) in DCM (0.5 ml) and stirred at room temp for 1 h. After 1 h, 2 drops of methanol and then NaHCO3 solution (5 ml) and ethyl acetate (30 ml) were added. The product was extracted into the ethyl acetate which was dried (Na2SO4) and concentrated. Purification by high pH MDAP gave desired product as a white solid in 44 mg.

WORKUP

后处理

  1. waitAfter 1 h
  2. extractionThe product was extracted into the ethyl acetate which
  3. dry with materialwas dried (Na2SO4)
  4. concentrationconcentrated
  5. customPurification by high pH