6-fluoro-1,4-oxazepane

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: The crude mixture (2.2 g) obtained by the previous procedure, which contained mainly (3R)-4-benzyl-3-fluoromethylmorpholine and 4-benzyl-6-fluoroperhydro-1,4-oxazepine, was dissolved in methanol (50 ml). The solution was hydrogenated in the presence of 10% palladium-carbon (200 mg) at room temperature. After 1 hour of stirring, palladium-carbon was removed by filtration and the filtrate was evaporated under reduced pressure. The two isomers were separated by column chromatography using 2% of methanol in dichloromethane as an eluent to give (3R)-3-fluoromethylmorpholine and 6-fluoroperhydro-1,4-oxazepine (the former was less polar). The products were converted to their hydrochloride as a conventional manner using 4N hydrogen chloride in ethyl acetate, respectively. palladium-carbon was removed by filtration the filtrate was evaporated under reduced pressure The two isomers were separated by column chromatography

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: The crude mixture (2.2 g) obtained by the previous procedure, which contained mainly (3R)-4-benzyl-3-fluoromethylmorpholine and 4-benzyl-6-fluoroperhydro-1,4-oxazepine, was dissolved in methanol (50 ml). The solution was hydrogenated in the presence of 10% palladium-carbon (200 mg) at room temperature. After 1 hour of stirring, palladium-carbon was removed by filtration and the filtrate was evaporated under reduced pressure. The two isomers were separated by column chromatography using 2% of methanol in dichloromethane as an eluent to give (3R)-3-fluoromethylmorpholine and 6-fluoroperhydro-1,4-oxazepine (the former was less polar). The products were converted to their hydrochloride as a conventional manner using 4N hydrogen chloride in ethyl acetate, respectively. palladium-carbon was removed by filtration the filtrate was evaporated under reduced pressure The two isomers were separated by column chromatography

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: The crude mixture (2.2 g) obtained by the previous procedure, which contained mainly (3R)-4-benzyl-3-fluoromethylmorpholine and 4-benzyl-6-fluoroperhydro-1,4-oxazepine, was dissolved in methanol (50 ml). The solution was hydrogenated in the presence of 10% palladium-carbon (200 mg) at room temperature. After 1 hour of stirring, palladium-carbon was removed by filtration and the filtrate was evaporated under reduced pressure. The two isomers were separated by column chromatography using 2% of methanol in dichloromethane as an eluent to give (3R)-3-fluoromethylmorpholine and 6-fluoroperhydro-1,4-oxazepine (the former was less polar). The products were converted to their hydrochloride as a conventional manner using 4N hydrogen chloride in ethyl acetate, respectively. palladium-carbon was removed by filtration the filtrate was evaporated under reduced pressure The two isomers were separated by column chromatography