反应详情

A solution of 25 mg (0.6 mmol) of LiOH.H2O in 0.4 ml of H2O is added dropwise to a suspension of 95 mg (0.30 mmol) of 4-(3-chloroanilino)-6-ethoxy-carbonyl-7H-pyrrolo[2,3-d]pyrimidine (see stage1.4) in 0.7 ml of methanol and the mixture is heated to boiling for 4.5 h. It is cooled in an ice bath and acidified with 0.6 ml of 1 normal HCl solution. Filtering off and washing with water yields 6-carboxy-4-(3-chloroanilino)-7H-pyrrolo[2,3-d]pyrimidine; HPLC: tRet(Grad20)=8.7; FAB-MS: (M+H)+=289.

1. temperaturethe mixture is heated
2. temperatureIt is cooled in an ice bath
3. filtrationFiltering off
4. washwashing with water