反应详情

(+/−) Tert-butyl (2-chloro-5-cyano-3-(3-(morpholine-4-carbonyl)-4-(oxetan-3-yl)piperazin-1-yl)phenyl)carbamate (112 mg, 0.221 mmol) was taken up in DCM (3 mL) and TFA (0.341 mL, 4.43 mmol) was added. The reaction was stirred at room temperature for 1 h. The solvent was removed in vacuo and the material was azeotroped 2× with DCM and 2× with MeOH, and then dried under vacuum. The solid was dissolved in EtOAc, and then washed with 2M K3PO4 solution. The organic layer was dried over Na2SO4, filtered, and concentrated. The material was purified by flash column chromatography (0-5% MeOH/DCM). (+/−) 3-amino-4-chloro-5-(3-(morpholine-4-carbonyl)-4-(oxetan-3-yl)piperazin-1-yl)benzonitrile (36 mg) was obtained as a colorless foam.

1. customThe solvent was removed in vacuo
2. customthe material was azeotroped 2× with DCM and 2× with MeOH
3. customdried under vacuum
4. dissolutionThe solid was dissolved in EtOAc
5. washwashed with 2M K3PO4 solution
6. dry with materialThe organic layer was dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated
9. customThe material was purified by flash column chromatography (0-5% MeOH/DCM)