反应详情

In a bomb tube, 155 mg (0.50 mmol) of 6-ethoxycarbonyl-4-[1(R)-phenyl-ethylamino]-7H-pyrrolo[2,3-d]pyrimidine and 2.5 mg (0.05 mmol) of NaCN in 4 ml of methylamine (33% in ethanol) are heated at 50° C. for 30 hours. The reaction mixture is dissolved in THF, 25 ml of water are added thereto and concentration by evaporation is carried out to a residual volume of =25 ml. The resulting crystals are filtered off and washed with water. Recrystallization from hot THF and ethyl acetate yields the title compound; HPLC: tRet (Grad20)=8.3; TLC-Rf =0.31 (CH2Cl2 /methanol [10:1]); FAB-MS: (M+H)+ =296.

1. concentrationconcentration
2. customby evaporation
3. filtrationThe resulting crystals are filtered off
4. washwashed with water
5. customRecrystallization from hot THF and ethyl acetate