2-氨基环己酮盐酸盐

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Dissolve 2-amino-cyclohexanone hydrochloride (2.2 g, 14.7 mmol) and potassium thiocyanate (1.4 g, 14.7 mmol) in water (10 mL). Stir the solution at 100° C. in a sealed flask for 16 h. Cool the mixture and store the mixture at 4° C. for 16 h. Filter off the resulting solid and wash with water (20 mL). Collect the solid, slurry in diethyl ether (20 mL) and filter. Dry the solid in a vacuum oven at 50° C. for 2 h to obtain the title compound as a tan solid (1.4 g, 62%). MS (ES+) m/z: 155.1 (M+H)+. Cool the mixture and store the mixture at 4° C. for 16 h Filter off the resulting solid wash with water (20 mL) Collect the solid slurry in diethyl ether (20 mL) and filter Dry the solid in a vacuum oven at 50° C. for 2 h

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

实验步骤: Add 2-nitrocyclohexanone (7.0 g, 48.9 mmol), 5% platinum sulfided on carbon (500 mg), ethanol (120 mL) and concentrated hydrochloric acid (6 mL) to a pressure vessel under a nitrogen atmosphere. Pressurize the vessel to 50 psi with hydrogen and stir the mixture for 3 h. Filter the mixture through Celite® and wash with ethanol followed by DCM under a nitrogen atmosphere. Concentrate the filtrate in vacuo. Slurry the residue in acetone (50 mL) and filter. Collect the solid to obtain the desired intermediate (2.2 g, 40%). Filter the mixture through Celite® wash with ethanol Concentrate the filtrate in vacuo filter Collect the solid

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

实验步骤: 6.00 g 4-Methoxy-7-morpholin-4-yl-benzothiazole-2-carboxylic acid and 3.75 g 1,1′-carbonyl-diimidazole in 360 ml dimethylformamide were stirred at room temperature for 16 hours. 3.36 g 2-amino-cyclohexanone hydrochloride and 3.14 ml triethylamine were added and stirring was continued over night at room temperature. Water was added and the mixture was extracted with ethylacetate. Chromatography on silicagel with ethylacetate/hexane 1:1 to yielded 0.16 g (2%) 4-methoxy-7-morpholin-4-yl-benzothiazole-2-carboxylic acid (2-oxo-cyclohexyl)-amide as a yellow solid; M.p.: 195–197° C.; MS (ISP): m/e=390 (M+H+). was continued over night at room temperature the mixture was extracted with ethylacetate