异丙托溴铵杂质13

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: 2M Hydrochloric acid (8 drops) was added to a stirred solution of 2,5-dimethoxytetrahydrofuran (16.5 g) in water (70 ml). After 15 minutes a mixture of diisopropylamine (7.38 g) and 2M hydrochloric acid (40 ml) was added to the reaction followed by acetonedicarboxylic acid (18.25 g) and sodium acetate (10.0 g) in water (100 ml). After 3 days 1,3-acetonedicarboxylic acid (6.0 g) and sodium acetate (3.0 g) were added. After a further 6 days the mixture was basified to pH8 and extracted with ethyl acetate. The extracts were dried (MgSO4) and evaporated under reduced pressure. The aqueous fraction was then extracted with chloroform and the extracts dried (MgSO4) and evaporated under reduced pressure. Distillation of the combined extracts (95-115° C.; 18 mmHg) gave 8-isopropyl-8-azabicyclo[3.2.1]octan-3-one (3.37 g). was added to the reaction extracted with ethyl acetate The extracts were dried (MgSO4) evaporated under reduced pressure The aqueous fraction was then extracted with chloroform the extracts dried (MgSO4) evaporated under reduced pressure Distillation of the combined extracts (95-115° C.; 18 mmHg)

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

实验步骤: 2M Hydrochloric acid (8 drops) was added to a stirred solution of 2,5-dimethoxytetrahydrofuran (16.5 g) in water (70 ml). After 15 minutes a mixture of diisopropylamine (7.38 g) and 2M hydrochloric acid (40 ml) was added to the reaction followed by acetonedicarboxylic acid (18.25 g) and sodium acetate (10.0 g) in water (100 ml). After 3 days 1,3-acetonedicarboxylic acid (6.0 g) and sodium acetate (3.0 g) were added. After a further 6 days the mixture was basified to pH8 and extracted with ethyl acetate. The extracts were dried (MgSO4) and evaporated under reduced pressure. The aqueous fraction was then extracted with chloroform and the extracts dried (MgSO4) and evaporated under reduced pressure. Distillation of the combined extracts (95-115° C.; 18 mmHg) gave 8-isopropyl-8-azabicyclo[3.2.1]octan-3-one (3.37 g). was added to the reaction extracted with ethyl acetate The extracts were dried (MgSO4) evaporated under reduced pressure The aqueous fraction was then extracted with chloroform the extracts dried (MgSO4) evaporated under reduced pressure Distillation of the combined extracts (95-115° C.; 18 mmHg)

反应条件: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 8-isopropyl-8-aza-bicyclo[3.2.1]octan-3-one (CAS 3423-28-7)(20.0 g, 120 mmol) in ethanol (500 ml) and pyridine (14.5 ml, 179 mmol) with hydroxylamine hydrochloride (8.81 g, 127 mmol) was refluxed for 16 h. Cooled to 23° C., the precipitate was filtered off, washed with diethyl ether leaving a solid, which was partitioned between dichloromethane and sodium carbonate solution, the organic layers dried over sodium sulfate, filtered and the solvents evaporated to give the title compound as a white solid. (17.7 g, 82%), MS: m/e=183.2 (M+H+). was refluxed for 16 h the precipitate was filtered off washed with diethyl ether leaving a solid, which was partitioned between dichloromethane and sodium carbonate solution the organic layers dried over sodium sulfate filtered the solvents evaporated

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

实验步骤: 2M Hydrochloric acid (8 drops) was added to a stirred solution of 2,5-dimethoxytetrahydrofuran (16.5 g) in water (70 ml). After 15 minutes a mixture of diisopropylamine (7.38 g) and 2M hydrochloric acid (40 ml) was added to the reaction followed by acetonedicarboxylic acid (18.25 g) and sodium acetate (10.0 g) in water (100 ml). After 3 days 1,3-acetonedicarboxylic acid (6.0 g) and sodium acetate (3.0 g) were added. After a further 6 days the mixture was basified to pH8 and extracted with ethyl acetate. The extracts were dried (MgSO4) and evaporated under reduced pressure. The aqueous fraction was then extracted with chloroform and the extracts dried (MgSO4) and evaporated under reduced pressure. Distillation of the combined extracts (95-115° C.; 18 mmHg) gave 8-isopropyl-8-azabicyclo[3.2.1]octan-3-one (3.37 g). was added to the reaction extracted with ethyl acetate The extracts were dried (MgSO4) evaporated under reduced pressure The aqueous fraction was then extracted with chloroform the extracts dried (MgSO4) evaporated under reduced pressure Distillation of the combined extracts (95-115° C.; 18 mmHg)

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 8-isopropyl-8-aza-bicyclo[3.2.1]octan-3-one (CAS no: 3423-28-7) (20.0 g, 120 mmol) in ethanol (500 mL) and pyridine (14.5 mL, 179 mmol) with hydroxylamine hydrochloride (8.81 g, 127 mmol) was refluxed for 16 h. Cooled to 23° C., the precipitate was filtered off, washed with diethyl ether leaving a solid, which was partitioned between dichloromethane and sodium carbonate solution, the organic layers dried over Na2SO4, filtered and the solvents evaporated to give the title compound as a white solid. (17.7 g, 82%); MS: m/e=183.2 (M+H+). the precipitate was filtered off washed with diethyl ether leaving a solid, which was partitioned between dichloromethane and sodium carbonate solution the organic layers dried over Na2SO4 filtered the solvents evaporated

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

实验步骤: 2M Hydrochloric acid (8 drops) was added to a stirred solution of 2,5-dimethoxytetrahydrofuran (16.5 g) in water (70 ml). After 15 minutes a mixture of diisopropylamine (7.38 g) and 2M hydrochloric acid (40 ml) was added to the reaction followed by acetonedicarboxylic acid (18.25 g) and sodium acetate (10.0 g) in water (100 ml). After 3 days 1,3-acetonedicarboxylic acid (6.0 g) and sodium acetate (3.0 g) were added. After a further 6 days the mixture was basified to pH8 and extracted with ethyl acetate. The extracts were dried (MgSO4) and evaporated-under reduced pressure. The aqueous fraction was then extracted with chloroform and the extracts dried (MgSO4) and evaporated under reduced pressure. Distillation of the combined extracts (95-115° C.; 18mmHg) gave 8-isopropyl-8-azabicyclo[3.2. 1]octan-3-one (3.37 g). was added to the reaction extracted with ethyl acetate The extracts were dried (MgSO4) The aqueous fraction was then extracted with chloroform the extracts dried (MgSO4) evaporated under reduced pressure Distillation of the combined extracts (95-115° C.; 18mmHg)

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

实验步骤: 2M Hydrochloric acid (8 drops) was added to a stirred solution of 2,5-dimethoxytetrahydrofuran (16.5 g) in water (70 ml). After 15 minutes a mixture of diisopropylamine (7.38 g) and 2M hydrochloric acid (40 ml) was added to the reaction followed by acetonedicarboxylic acid (18.25 g) and sodium acetate (10.0 g) in water (100 ml). After 3 days 1,3-acetonedicarboxylic acid (6.0 g) and sodium acetate (3.0 g) were added. After a further 6 days the mixture was basified to pH8 and extracted with ethyl acetate. The extracts were dried (MgSO4) and evaporated under reduced pressure. The aqueous fraction was then extracted with chloroform and the extracts dried (MgSO4) and evaporated under reduced pressure. Distillation of the combined extracts (95-115° C.; 18 mmHg) gave 8-isopropyl-8-azabicyclo[3.2.1]octan-3-one (3.37 g). was added to the reaction extracted with ethyl acetate The extracts were dried (MgSO4) evaporated under reduced pressure The aqueous fraction was then extracted with chloroform the extracts dried (MgSO4) evaporated under reduced pressure Distillation of the combined extracts (95-115° C.; 18 mmHg)