反应详情

13.1 g of N-(trans-4-methylcyclohexyl ) -4-dimethylaminobutylamide (Example 73) was dissolved in 100 ml of THF. Under an argon stream, the solution was added dropwise to a solution of 7.5 g of lithium aluminum hydride suspended in 400 ml of THF under ice-cooling. After the addition, the solution was reacted for 8 hours, while it was refluxed. After reaction, the solution was allowed to cool to room temperature. Then, 22 g of sodium sulfate decahydrate was added to the solution under ice-cooling. The solution was stirred for 1 hour, and the precipitate was filtered out. The solvent was removed in vacuo, yielding an oily substance. This substance was subjected to vacuum distillation, yielding 5.7 g of N-(4-dimethylaminobutyl)-trans-4-methylcyclohexylamine as a colorless oil, which had the following physiochemical properties:

1. temperaturecooling
2. additionAfter the addition
3. customthe solution was reacted for 8 hours, while it
4. temperaturewas refluxed
5. customAfter reaction
6. temperaturecooling
7. filtrationthe precipitate was filtered out
8. customThe solvent was removed in vacuo
9. customyielding an oily substance
10. distillationThis substance was subjected to vacuum distillation