HRID1486572
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
To a solution of tert-butyl 5-((3-(3,5-dichlorophenylamino)-1H-1,2,4-triazol-5-ylamino)methyl)pyridin-2-ylcarbamate Compound 6 (50 mg, 111 μmol) in DCM (1 ml) was added TFA (1 ml) and the reaction was stirred for 1 hour. The reaction mixture was concentrated in vacuo and was partitioned between DCM (5 ml) and sat. NaHCO3 (3 ml). The layers were separated and the aqueous layer was extracted with DCM (3×5 ml). The combined organic solution was washed with brine (5 ml), dried over Na2SO4, filtered and concentrated to give a white solid as desired product (10.2 mg, 26% yield). MS +m/z: 350 (M+H)+
WORKUP
后处理
- concentrationThe reaction mixture was concentrated in vacuo
- customwas partitioned between DCM (5 ml) and sat. NaHCO3 (3 ml)
- customThe layers were separated
- extractionthe aqueous layer was extracted with DCM (3×5 ml)
- washThe combined organic solution was washed with brine (5 ml)
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated