反应详情

90 mg (0.285 mmol) of 4-(3-chloroanilino)-6-ethoxycarbonyl-7H-pyrrolo-[2,3-d]pyrimidine (stage 1.4) in 30 ml of methanol and≈5 g of ammonia are heated at 120° C. for 48 h in an autoclave. The reaction mixture is treated with silica gel, evaporated, applied to a silica gel column as a powder and finally eluted with methylene chloride/methanol/THF (210:35:10). Filtration with methanol through an alumina column (basic) and stirring in ethyl acetate yields 6-aminocarbonyl-4-(3-chloroanilino)-7H-pyrrolo[2,3-d]pyrimidine; HPLC: tRet(Grad20)=8.1; TLC-Rf=0.18 (CH2Cl2/methanol [10:1]); high resolution MS: (M+H)+=288.0669 (calc. 288.0652).

1. additionThe reaction mixture is treated with silica gel
2. customevaporated
3. washfinally eluted with methylene chloride/methanol/THF (210:35:10)
4. filtrationFiltration with methanol through an alumina column (basic)