反应详情

A mixture of 1.58 g of 6-[[(4-butylphenyl)methyl]amino]-1-hexanol and 1.5 g of phenyl-N-(2,4-difluorophenyl)carbamate in 40 ml of toluene was heated at reflux for 5 hours. The reaction mixture was cooled and allowed to stand at room temperature for 16 hours. The solution was washed with 3N aqueous hydrochloric acid, brine, 1N aqueous sodium hydroxide and brine again, then was dried over anhydrous magnesium sulfate and filtered. The filtrate was evaporated in vacuo and gave a yellow oil. The oil was treated by preparative high pressure liquid chromatography and gave 0.93 g (37%) of the desired product as a colorless oil.

1. temperaturewas heated
2. temperatureat reflux for 5 hours
3. temperatureThe reaction mixture was cooled
4. washThe solution was washed with 3N aqueous hydrochloric acid, brine, 1N aqueous sodium hydroxide and brine again
5. dry with materialwas dried over anhydrous magnesium sulfate
6. filtrationfiltered
7. customThe filtrate was evaporated in vacuo
8. customgave a yellow oil
9. additionThe oil was treated by preparative high pressure liquid chromatography