反应详情

Formic acid (0.25 ml, 6.63 mmol) was added dropwise to a solution of 1-benzyl-N-trityl-3-azepanamine (300 mg, 0.672 mmol) in methylene chloride (7 ml) under ice-cooling and stirred under ice-cooling for 3.5 hours. After the reaction mixture was concentrated, the residue was diluted with ether and washed with 1N-hydrochloric acid. After extraction, a 1N-aqueous sodium hydroxide solution was added to the aqueous layer under ice-cooling to make the aqueous layer basic, followed by extraction with chloroform. The organic layer was dried over magnesium sulfate and then concentrated to obtain 1-benzyl-3-azepanamine (100 mg, 73%).

1. temperaturecooling
2. temperaturecooling for 3.5 hours
3. concentrationAfter the reaction mixture was concentrated
4. additionthe residue was diluted with ether
5. washwashed with 1N-hydrochloric acid
6. extractionAfter extraction
7. additiona 1N-aqueous sodium hydroxide solution was added to the aqueous layer under ice-
8. temperaturecooling
9. extractionfollowed by extraction with chloroform
10. dry with materialThe organic layer was dried over magnesium sulfate
11. concentrationconcentrated