HRID854253

反应详情

EQUATION

反应方程式

HRID 854253 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

709 mg of 4-[4-((2S)-2-benzyloxycarbonylamino-2-tert-butoxycarbonyl-ethylamino)-2-methyl-pyrrolo[2,3-d]pyrimidin-7-yl]-butyric acid ethyl ester were dissolved in 40 ml of ethanol and 1 ml of acetic acid and were hydrogenated over 100 mg of Pd/C (10%) during 4 h at room temperature. The catalyst was removed by filtration, the solvent was removed in vacuo. The residue was dissolved in 60 ml of DCM and stirred with 10 ml of brine and additional 5 g of NaHCO3. The phases were separated, the aqueous phase was extracted with DCM, the combined organic phases were dried over MgSO4, filtered and the solvent was removed in vacuo. Yield: 475 mg.

WORKUP

后处理

  1. customThe catalyst was removed by filtration
  2. customthe solvent was removed in vacuo
  3. dissolutionThe residue was dissolved in 60 ml of DCM
  4. customThe phases were separated
  5. extractionthe aqueous phase was extracted with DCM
  6. dry with materialthe combined organic phases were dried over MgSO4
  7. filtrationfiltered
  8. customthe solvent was removed in vacuo