HRID1959359

反应详情

EQUATION

反应方程式

HRID 1959359 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Tert-butyl-4-[5-amino-6-(2-pyridylcarbamoyl)pyrazin-2-yl]piperazine-1-carboxylate (5.43 g, 13.59 mmol) was suspended in DCM (50 mL) and stirred at 0° C. during addition of TFA (10 ml). The reaction mixture was warmed to RT over 2 hours but analysis showed little deprotection. The reaction was treated with a further 30 ml of TFA and stirred at RT for 15 minutes. The mixture was concentrated under reduced pressure to give a dark red oil which was dissolved in MeOH/DCM and azeotroped with toluene to give an intense orange solid which was filtered, washed with ether and dried under high vacuum (5.41 g, 73% Yield).

WORKUP

后处理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customto give a dark red oil which
  3. customazeotroped with toluene
  4. customto give an intense orange solid which
  5. filtrationwas filtered
  6. washwashed with ether
  7. customdried under high vacuum (5.41 g, 73% Yield)