HRID51500

反应详情

EQUATION

反应方程式

HRID 51500 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of ethyl 2-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]propionate (201 mg), aqueous potassium hydroxide solution (4 ml of 2M solution) and methanol (20 ml) was boiled under reflux for 1 hour. The mixture was concentrated under reduced pressure to around 5 ml and then diluted with water (30 ml). The mixture was hot filtered and filtrate was cooled and then acidified with dilute acetic acid until no further precipitation occurred. The mixture was heated on a hot plate until the gel which had been obtained became a finely divided solid. The solid was collected by filtration to give 2-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]propionic acid, m.p. 239.5-241° C.

WORKUP

后处理

  1. temperatureunder reflux for 1 hour
  2. concentrationThe mixture was concentrated under reduced pressure to around 5 ml
  3. additiondiluted with water (30 ml)
  4. filtrationThe mixture was hot filtered
  5. temperaturefiltrate was cooled
  6. customacidified with dilute acetic acid until no further precipitation
  7. temperatureThe mixture was heated on a hot plate until the gel which
  8. customhad been obtained
  9. filtrationThe solid was collected by filtration