反应详情

To a cooled (0° C.) solution of tert-butyl 3-((2,4-difluorophenyl)amino)azetidine-1-carboxylate (D31) (90 mg, 0.316 mmol) in dichloromethane, a mixture of trifluoroacetic acid/dichloromethane (3 ml/1 ml) was added and the reaction mixture was stirred 1 h. The solvents were evaporated in vacuo and the residue was dissolved in tetrahydrofuran/methanol (3/1 ml) triethylamine (0.132 ml, 0.95 mmol) was added followed by the addition of methyl 2,5-dichloronicotinate (52.33 mg, 0.253 mmol) and the resulting mixture was stirred 12 h at 75° C. The residue abtained after solvent evaporation was purified by Biotage SNAP-Si column eluting with cyclohexane/ethyl acetate from 100/0 to 90/10. Collected fractions afforded the title compound (D85) (0022/086/5) (38 mg).

1. additionwas added
2. customThe solvents were evaporated in vacuo
3. additionwas added
4. stirringthe resulting mixture was stirred 12 h at 75° C
5. customafter solvent evaporation
6. customwas purified by Biotage SNAP-Si column
7. washeluting with cyclohexane/ethyl acetate from 100/0 to 90/10