反应详情

69.3 mg (0.83 mmol) of O-methylhydroxylamine hydrochloride and 69.3 mg (0.845 mmol) of sodium acetate in 1 ml of water are added to 163.3 mg (0.5 mmol) of 4-(3-chloroanilino)-6-formyl-7H-pyrrolo[2,3-d]pyrimidine (stage1.6) in 1 ml of methanol. The suspension is heated to boiling for 4 h, cooled and filtered, and the residue is washed with water/isopropanol and finally diethyl ether. 4-(3-Chloroanilino)-7H-pyrrolo[2,3-d]pyrimidine-6-carbaldehyde O-methyl oxime is obtained; HPLC: tRet(Grad20)=11.3; TLC-Rf=0.31 (CH2Cl2/methanol 10:1) FAB-MS: (M+H)+=302.

1. temperatureThe suspension is heated
2. temperaturecooled
3. filtrationfiltered
4. washthe residue is washed with water/isopropanol and finally diethyl ether