HRID19401

反应详情

EQUATION

反应方程式

HRID 19401 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

[(S)-3-Methyl-1-(pyrazin-2-ylcarbamoyl)-butyl]-carbamic acid t-butyl ester (0.645 g, 2.09 mmol) was treated with a 30% trifluoroacetic acid/dichloromethane (10 mL) solution at 0° C. and the resulting mixture allowed to warm to room temperature over 1.5 h. At this time the mixture was partioned between ethyl acetate and water and the layers separated. The aqueous phase was made basic (pH=10) by the addition of solid sodium hydroxide. The basic aqueous phase was extracted with ethyl acetate (3×) and the ethyl acetate layers were combined, dried over sodium sulfate, filtered and concentrated in vacuo to afford (S)-2-amino-4-methyl-pentanoic acid pyrazin-2-ylamide (0.341 g, 78%).

WORKUP

后处理

  1. customthe layers separated
  2. additionby the addition of solid sodium hydroxide
  3. extractionThe basic aqueous phase was extracted with ethyl acetate (3×)
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo