反应详情

109 mg (0.40 mmol) of 4-(3-chloroanilino)-6-formyl-7H-pyrrolo[2,3-d]pyrimidine (stage 1.6) and 84 mg (0.8 mmol) of diethanolamine in 6 ml of ethanol, 60 drops of DMPU and 50 μl of acetic acid are stirred at RT for a few hours. 30 mg of Raney nickel are then added and the mixture is hydrogenated at 50° C. The catalyst is filtered off and the filtrate is evaporated. Column chromatography (SiO2, CH2Cl2/methanol=10:1) and crystallization from ethyl acetate/diethyl ether yields 4-(3-chloroanilino)-6-[bis(2-hydroxyethyl)aminomethyl]-7H-pyrrolo[2,3-d]pyrimidine; HPLC: tRet(Grad20)=7.0; TLC-Rf=0.1 (CH2Cl2/methanol=10:1); FAB-MS: (M+H)+=362.

1. customis hydrogenated at 50° C
2. filtrationThe catalyst is filtered off
3. customthe filtrate is evaporated
4. customColumn chromatography (SiO2, CH2Cl2/methanol=10:1) and crystallization from ethyl acetate/diethyl ether