反应详情

To a solution of 20 g (63.2 mmol) 5-(3-benzyloxy-phenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-ylamine (see WO 97/28161) in 1 l dry N,N-dimethylformamide, 12.4 g (69.5 mmol) N-bromosuccinimide are added at ca. 10° C. Stirring was continued at ca. 10° C. for 30 min and overnight at RT. The precipitate formed is filtered off and washed thoroughly with N,N-dimethylformamide and hexane. After drying for 24 h at 30-35° C. under vacuum, the title compound is used in the next step without further purification. Additional material can be obtained from the mother liquor through chromatography on silicagel. Analytical HPLC: tR=10.07 min (Grad 1); ES-MS: m/eo=394.9 and 396.9; NMR (DMSO-d6): 12.55/s (NH); 8.06/s (1H), 7.25-7.5/several m's (6H), 7.07/“d” (1H); 7.03/s (1H); 6.98/“d” (1H); 5.5-6.0/b (NH2); 5.12/s (2H).

1. customThe precipitate formed
2. filtrationis filtered off
3. washwashed thoroughly with N,N-dimethylformamide and hexane
4. customAfter drying for 24 h at 30-35° C. under vacuum
5. customthe title compound is used in the next step without further purification
6. customAdditional material can be obtained from the mother liquor through chromatography on silicagel