2(1H)-Quinoxalinone,octahydro-,(4aR,8aS)-rel-(9CI)

反应条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: (+/−)-cis-Decahydroquinoxalin-2-one (0.8 g, 5.19 mmol) is suspended in 25 ml of H2O. NaHCO3 (0.87 g, 10.35 mmol) is added and the reaction mixture is cooled to 10° C. Benzylchloroformate (1 ml, 6.68 mmol) is added dropwise to the vigorously stirred mixture. After 20 hours at room temperature the solid is filtered, washed thoroughly with H2O, air-dried. The title compound (1.46 g, 98% yield) is obtained as a white solid. After 20 hours at room temperature the solid is filtered washed thoroughly with H2O air-dried

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: cis-1,2-Diaminocyclohexane (4.1 g, 36 mmol) is dissolved in 150 ml of H2O. Chloroacetic acid (3.4 g, 36 mmol) in 50 ml of H2O is added dropwise at 10° C. in 5 minutes, then potassium carbonate (7.9 g, 57 mmol) in 30 ml of H2O is added dropwise at 10 C. The reaction mixture is allowed to warm slowly to room temperature and stirred 24 hours. The solution is heated at 90° C. for 2 hours, concentrated. The resulting solid is taken-up in boiling toluene (100 ml), filtered while hot, concentrated to give (+/−)-cis-decahydroquinoxalin-2-one (0.8 g, 14% yield) as a white solid. The solution is heated at 90° C. for 2 hours concentrated filtered while hot, concentrated

反应条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: (+/−)-cis-decahydroquinoxalin-2-one (0.8 g, 5.19 mmol) is suspended in 25 ml of H2O. NaHCO3 (0.87 g, 10.35 mmol) is added and the reaction mixture is cooled to 10° C. Benzylchloroformate (1 ml, 6.68 mmol) is added dropwise to the vigorously stirred mixture. After 20 hours at room temperature the solid is filtered, washed thoroughly with H2O, air-dried. The title compound (1.46 g, 98% yield) is obtained as a white solid. C16H20N2O3, MS (M+H)+:289 After 20 hours at room temperature the solid is filtered washed thoroughly with H2O air-dried

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: cis-1,2-Diaminocyclohexane (4.1 g, 36 mmol) is dissolved in 150 ml of H2O. Chloroacetic acid (3.4 g, 36 mmol) in 50 ml of H2O is added dropwise at 10° C. in 5 minutes, then potassium carbonate (7.9 g, 57 mmol) in 30 ml of H2O is added dropwise at 10 C. The reaction mixture is allowed to warm slowly to room temperature and stirred 24 hours. The solution is heated at 90° C. for 2 hours, concentrated. The resulting solid is taken-up in boiling toluene (100 ml), filtered while hot, concentrated to give (+/−)-cis-decahydroquinoxalin-2-one (0.8 g, 14% yield) as a white solid. C8H14N2O, MS (M+H)+: 155 The solution is heated at 90° C. for 2 hours concentrated filtered while hot, concentrated