反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder reflux for 1 hour
- concentrationThe mixture was concentrated under reduced pressure to around 5 ml
- additiondiluted with water (30 ml)
- filtrationThe mixture was hot filtered
- temperaturefiltrate was cooled
- customacidified with dilute acetic acid until no further precipitation
- temperatureThe mixture was heated on a hot plate until the gel which
- customhad been obtained
- filtrationThe solid was collected by filtration