HRID251732

反应详情

EQUATION

反应方程式

HRID 251732 的结构方程式

PROCEDURE

实验过程

A solution of (2S)-2-[(tert-butoxycarbonyl)amino]-8-oxodecanoic acid, EDC.HCl (1.3 eq.) and HOBt (1.3 eq.) in DMF was shaken for 5 min. To the mixture was added a solution of crude amine (L2) (1 eq.) and DIPEA (1 eq.) in DMF. The mixture was left to stir for 1 h. It was partitioned between DMF and 1 M NaOH. The DCM phase was washed sequentially with 1 M NaOH, 1 M HCl and brine, dried (Na2SO4) and concentrated under reduced pressure. The residue was purified by chromatography on silica using 50% EtOAc/Petroleum ether as eluent to yield the product was obtained as a colourless oil. MS (ES) C27H36N2O5 requires: 468, found: 469 (M+H)+.

WORKUP

后处理

  1. waitThe mixture was left
  2. customIt was partitioned between DMF and 1 M NaOH
  3. washThe DCM phase was washed sequentially with 1 M NaOH, 1 M HCl and brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by chromatography on silica using 50% EtOAc/Petroleum ether as eluent
  7. customto yield the product
  8. customwas obtained as a colourless oil