HRID1180094
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 mixture of 2-(2-Amino-pyrimidin-4-yl)-4-oxo-1,4,6,7-tetrahydro-pyrrolo[3,2-c]pyridine-5-carboxylic acid tert-butyl ester and Et3N (4 eq.) in dry THF, PhCOCl (2 eq.) was added and the mixture was stirred at room temperature under argon overnight. Thus NaOH(1N) was added; after 30′ the solvent was evaporated and the residue was dissolved in water and the aqueous phase was extracted with AcOEt (2×). The organic phase was then washed with aq. NH4Cl and dried over Na2SO4. After solvent evaporation the crude product was purified by flash chromatography (CH2Cl2:MeOH 97:3) to give the pure product as a solid.
WORKUP
后处理
- additionwas added
- customafter 30′ the solvent was evaporated
- dissolutionthe residue was dissolved in water
- extractionthe aqueous phase was extracted with AcOEt (2×)
- washThe organic phase was then washed with aq. NH4Cl
- dry with materialdried over Na2SO4
- customAfter solvent evaporation the crude product
- customwas purified by flash chromatography (CH2Cl2:MeOH 97:3)