HRID352175

反应详情

EQUATION

反应方程式

HRID 352175 的结构方程式

PROCEDURE

实验过程

S-amino enantiomer of N-({3-[(t-butoxy)carbonyl-amino]cyclohexyl}methyl) (phenylmethoxy)carboxamide (1.0 g, 2.76 mmol) was treated with TFA (5 mL) under N2. After 20 min of stirring at r.t. the reaction was complete. The crude was then concentrated to an oil which was purified on a Varian Bond-Elut SCX column (10 g). The column was eluted consecutively with CHCl3, MeOH, and ammonia (2.0M in MeOH). The pure product was recovered from the ammonia fractions. The solvent was removed in vacuo to afford 0.632 g (87%) as a colorless oil. MS (ES+) m/z 263.0 (M+H)+.

WORKUP

后处理

  1. concentrationThe crude was then concentrated to an oil which
  2. customwas purified on a Varian Bond-Elut SCX column (10 g)
  3. washThe column was eluted consecutively with CHCl3, MeOH, and ammonia (2.0M in MeOH)
  4. customThe pure product was recovered from the ammonia fractions
  5. customThe solvent was removed in vacuo
  6. customto afford 0.632 g (87%) as a colorless oil