HRID1697406

反应详情

EQUATION

反应方程式

HRID 1697406 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

To 3-[3-{[1-(2-{[2-(Benzyloxy)ethyl]sulfanyl}phenyl)-1-methylethyl]amino}-5-bromo-2-oxopyrazin-1(2H)-yl]-N-cyclopropyl-5-fluoro-4-methylbenzamide (Example 320e, 1.7 g) in ethanol (35 mL) was added ammonium formate (2.255 g) and Pd/C (0.544 g) and the resulting solution heated at 75° C. for 1 h. After cooling to room temperature, type 490 paste 10% Pd/C (0.272 g) slurried in ethanol (5 mL) was added and the reaction heated to 75° C. for 1 hr. The reaction was filtered through celite then the filtrate concentrated in vacuo then extracted into DCM. The organic solution was dried (MgSO4) and concentrated in vacuo to give the sub title compound (1.290 g).

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. additionwas added
  3. temperaturethe reaction heated to 75° C. for 1 hr
  4. filtrationThe reaction was filtered through celite
  5. concentrationthe filtrate concentrated in vacuo
  6. extractionthen extracted into DCM
  7. dry with materialThe organic solution was dried (MgSO4)
  8. concentrationconcentrated in vacuo