HRID1180094

反应详情

EQUATION

反应方程式

HRID 1180094 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas added
  2. customafter 30′ the solvent was evaporated
  3. dissolutionthe residue was dissolved in water
  4. extractionthe aqueous phase was extracted with AcOEt (2×)
  5. washThe organic phase was then washed with aq. NH4Cl
  6. dry with materialdried over Na2SO4
  7. customAfter solvent evaporation the crude product
  8. customwas purified by flash chromatography (CH2Cl2:MeOH 97:3)