HRID7321

反应详情

EQUATION

反应方程式

HRID 7321 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of benzyl (3R)-1-[(2S)-2-((3S)-3-{[(6-chloro-2-naphthyl)sulfonyl]amino}-2-oxopyrrolidin-1-yl)propanoyl]piperidin-3-ylcarbamate (0.350 g), 10% palladium on carbon (0.035 g) and ethanol (1000 ml) was stirred under an atmosphere of hydrogen for 17 h. The reaction mixture was filtered through Harbolite™ and the filtrate was concentrated under reduced pressure to give an oil. The oil was partially purified using SPE (silica, eluting with methanol and then 10% aqueous ammonia in methanol) and then fully purified using mass directed preparative h.p.l.c. to give the title compounds (Example 403, 0.01 g; Example 404, 0.028 g), both as oils.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through Harbolite™
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customto give an oil
  4. customThe oil was partially purified
  5. washeluting with methanol
  6. custom10% aqueous ammonia in methanol) and then fully purified