HRID1889109
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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 Dichloromethane (DCM) (1.5 mL) was treated with 2,3-dichlorobenzoyl chloride (55.3 mg, 0.264 mmol, commercially available) and stirred at room temp for 1 hr. After 1 hr, 2 drops of methanol and then NaHCO3 solution (5 ml) and ethyl acetate (30 ml) were added and the product was extracted into the ethyl acetate which was dried (Na2SO4) and concentrated. Purification by high pH MDAP gave desired material as a white solid in 76 mg.
WORKUP
后处理
- waitAfter 1 hr
- extractionthe product was extracted into the ethyl acetate which
- dry with materialwas dried (Na2SO4)
- concentrationconcentrated
- customPurification by high pH
- customMDAP gave desired material as a white solid in 76 mg