HRID6532

反应详情

EQUATION

反应方程式

HRID 6532 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 1.16 g of diethyl N-[4-{1-(tetrahydropyr-2-yloxy)-3-(4-hydroxy-6-pivaloylaminopyrrolo[2,3-d]pyrimidin-3-yl)prop-2-en-2-yl}benzoyl]glutamate and 174 mg (20%) of amorphous platinum (IV) oxide in 150 ml of glacial acetic acid is hydrogenated for 10 hours at 50 psi. The reaction mixture is diluted with 50 ml of methanol and filtered through Celite. The filtrate is concentrated and diluted with ethyl acetate. The solid which forms after cooling for 15 hour is collected by filtration, washed with cold ethyl acetate and dried to give diethyl N-[4-{1-(tetrahydropyr-2-yloxy)-3-(4-hydroxy-6-pivaloylaminopyrrolo[2,3-d]pyrimidin-3-yl)prop--2-yl}benzoyl]glutamate.

WORKUP

后处理

  1. filtrationfiltered through Celite
  2. concentrationThe filtrate is concentrated
  3. additiondiluted with ethyl acetate
  4. temperatureThe solid which forms after cooling for 15 hour
  5. filtrationis collected by filtration
  6. washwashed with cold ethyl acetate
  7. customdried