反应详情

To a solution of 1.96 g of 4-{[(1S,2R)-2-(cyanoamino)cyclohexyl]amino}-N-(2-methoxyethyl)-6-methylquinazolin-2-carboxamide and 8.56 g of methoxyamine hydrochloride in 80 ml of ethanol, 10.86 g of sodium carbonate was added and the mixture was heated at reflux for 1 hour. The reaction solution was added to 400 ml of ice water, and the deposited substance was collected by filtration. After the collected deposited substance was washed with water, it was dried under reduced pressure. The obtained powder was washed with a mixed solution of (chloroform:diisopropyl alcohol=1:1), whereby 1.71 g of a desired compound was obtained as a white powder.

1. temperaturethe mixture was heated
2. temperatureat reflux for 1 hour
3. filtrationthe deposited substance was collected by filtration
4. washAfter the collected deposited substance was washed with water, it
5. customwas dried under reduced pressure
6. washThe obtained powder was washed with a mixed solution of (chloroform:diisopropyl alcohol=1:1)