反应详情

A suspension of ((S)-5-benzyloxycarbonylamino-1-{[(3,5-diamino-6-chloro-pyrazine-2-carbonyl)-amino]-methyl}-pentyl)-carbamic acid tert-butyl ester (0.68 g, 1.27 mmol) in EtOH (20 mL) under an inert atmosphere of N2 is treated with activated palladium on charcoal (10%). The reaction mixture is then placed under a positive pressure of hydrogen and stirred at RT. After 3 h, the catalyst is removed by filtration through Celite® (filter material). The filtrate is concentrated in vacuo and the resulting colourless oil is dissolved in MeOH (10 mL) and allowed to stand at RT overnight. A cream precipitate forms which is removed by filtration and the solution is concentrated in vacuo. Purification by reverse phase column chromatography (Isolute™ C18, 0-100% acetonitrile in water with 0.1% NH3) affords the title compound. [M+H]+ 402.

1. customthe catalyst is removed by filtration through Celite® (filter material)
2. concentrationThe filtrate is concentrated in vacuo
3. dissolutionthe resulting colourless oil is dissolved in MeOH (10 mL)
4. waitto stand at RT overnight
5. customA cream precipitate forms which is removed by filtration
6. concentrationthe solution is concentrated in vacuo
7. customPurification by reverse phase column chromatography (Isolute™ C18, 0-100% acetonitrile in water with 0.1% NH3)