反应详情

温度

50 °C

Under a N2 atmosphere, 1.4 g (37 mmol) of lithium aluminum hydride are added in portions to 5.70 g (18 mmol) of 4-(3-chloroanilino)-6-ethoxycarbonyl-7H-pyrrolo[2,3-d]pyrimidine. After stirring at 50° C. for 2 h, 100 ml of water are added dropwise to the reaction mixture and it is filtered through Celite. Water is added to the filtrate and the mixture is extracted 3 times with ethyl acetate. The organic phases are washed 3 times with water and brine, dried (MgSO4) and evaporated. Recrystallization from isopropanol yields 4-(3-chloroanilino)-6-hydroxymethyl-7H-pyrrolo[2,3-d]pyrimidine; HPLC: tRet(Grad20)=8.2; TLC-Rf=0.11 (CH2Cl2/methanol [10:1]); MS: (M)+=274.

1. filtrationis filtered through Celite
2. additionWater is added to the filtrate
3. extractionthe mixture is extracted 3 times with ethyl acetate
4. washThe organic phases are washed 3 times with water and brine
5. dry with materialdried (MgSO4)
6. customevaporated
7. customRecrystallization from isopropanol