3-(4-溴-2-甲氧基苯氧基)氮杂环丁烷

反应条件: temp:0.00; pressure:0.00; stir:

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: Dissolve 3-(4-bromo-2-methoxy-phenoxy)-azetidine (1.84 g, 7.13 mmol) in dichloroethane (80 mL). Add cyclobutanone (1.86 mL, 25 mmol), sodium triacetoxyborohydride (3.02 g, 14.3 mmol) and acetic acid (0.82 mL, 14.3 mmol). Stir the mixture overnight, then add saturated sodium bicarbonate and extract three times using dichloromethane. Dry the combined organic portions over sodium sulfate, filter, and concentrate. Purify by silica gel chromatography using a 0-3% gradient of methanol/dichloromethane to give 1.26 g (56%) of the title compound. add saturated sodium bicarbonate and extract three times Dry the combined organic portions over sodium sulfate filter concentrate Purify by silica gel chromatography

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

实验步骤: Dissolve 3-(4-bromo-2-methoxy-phenoxy)-azetidine-1-carboxylic acid tert-butyl ester (2.9 g, 8.10 mmol) in dichloromethane (45 mL) and slowly add trifluoroacetic acid (15 mL). Stir the mixture for one hour and then evaporate. Apply the residue to two 10 g SCX columns with methanol. Wash the columns with methanol, then elute the material using 2N ammonia/methanol. Concentrate to give 2.09 g (88%) of the title compound as a clear oil. evaporate Wash the columns with methanol elute the material Concentrate

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

实验步骤: Dissolve 3-(4-bromo-2-methoxy-phenoxy)-azetidine-1-carboxylic acid tert-butyl ester (2.9 g, 8.10 mmol) in dichloromethane (45 mL) and slowly add trifluoroacetic acid (15 mL). Stir the mixture for one hour and then evaporate. Apply the residue to two 10 g SCX columns with methanol. Wash the columns with methanol, then elute the material using 2N ammonia/methanol. Concentrate to give 2.09 g (88%) of the title compound as a clear oil. evaporate Wash the columns with methanol elute the material Concentrate

反应条件: temp:0.00; pressure:0.00; stir:

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: Dissolve 3-(4-bromo-2-methoxy-phenoxy)-azetidine (1.84 g, 7.13 mmol) in dichloroethane (80 mL). Add cyclobutanone (1.86 mL, 25 mmol), sodium triacetoxyborohydride (3.02 g, 14.3 mmol) and acetic acid (0.82 mL, 14.3 mmol). Stir the mixture overnight, then add saturated sodium bicarbonate and extract three times using dichloromethane. Dry the combined organic portions over sodium sulfate, filter, and concentrate. Purify by silica gel chromatography using a 0-3% gradient of methanol/dichloromethane to give 1.26 g (56%) of the title compound. add saturated sodium bicarbonate and extract three times Dry the combined organic portions over sodium sulfate filter concentrate Purify by silica gel chromatography

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

实验步骤: Dissolve 3-(4-bromo-2-methoxy-phenoxy)-azetidine-1-carboxylic acid tert-butyl ester (2.9 g, 8.10 mmol) in dichloromethane (45 mL) and slowly add trifluoroacetic acid (15 mL). Stir the mixture for one hour and then evaporate. Apply the residue to two 10 g SCX columns with methanol. Wash the columns with methanol, then elute the material using 2N ammonia/methanol. Concentrate to give 2.09 g (88%) of the title compound as a clear oil. evaporate Wash the columns with methanol elute the material Concentrate