反应详情

7H-Indolo[2,1-a][2]benzazepine-10-carboxamide, 13-cyclohexyl-N-[(dimethylamino)sulfonyl]-6-[[4-(2-hydroxy-2-methyl-l-oxopropyl)-1-piperazinyl]carbonyl]-3-methoxy-. To a solution of tert-butyl piperazine-1-carboxylate (372 mg, 2.0 mmol), 2-hydroxy-2-methylpropanoic acid (229 mg, 2.2 mmol) and triethylamine (1.1 mL) in DMF (7 mL) was added HATU (988 mg, 2.6 mmol). The reaction mixture was stirred at rt for 2 h, then diluted with H2O, neutralized with 1N aqueous HCl (8 mL), concentrated, and the residue was partitioned between EtOAc and H2O. The organic phase was separated, washed with brine and concentrated to a white solid (1.1 g). The solid was dissolved into ClCH2CH2Cl (10 mL) and treated with trifluoroacetic acid (5 mL). The reaction mixture was stirred at rt for 2 h, and concentrated to yield crude 2-hydroxy-2-methyl-1-(piperazin-1-yl)propan-1-one (1.1 g) as yellow semi-solid.

1. concentrationconcentrated
2. customthe residue was partitioned between EtOAc and H2O
3. customThe organic phase was separated
4. washwashed with brine
5. concentrationconcentrated to a white solid (1.1 g)
6. dissolutionThe solid was dissolved into ClCH2CH2Cl (10 mL)
7. additiontreated with trifluoroacetic acid (5 mL)
8. stirringThe reaction mixture was stirred at rt for 2 h
9. concentrationconcentrated