反应详情

To a solution of trans-4-[N-[1-(cyanoimino)propyl]amino]-3,4-dihydro-2,2-dimethyl-3-hydroxy-2H-1-benzopyran-6-carbonitrile (1.49 g) in dry pyridine (7.5 ml) was added dropwise mesyl chloride (0.77 g) under ice-water cooling. The resulting mixture was stirred overnight at room temperature and concentrated under reduced pressure. The residue was dissolved in a mixture of ethyl acetate and washed with 5% hydrochloric acid (twice), aqueous sodium bicarbonate and brine, successively. The organic layer was dried over anhydrous magnesium sulfate and evaporated in vacuo. The residue was recrystallized from ethanol to give trans-4-[N-[1-(cyanoimino)propyl]amino]-3,4-dihydro-2,2-dimethyl-3-mesyloxy-2H-1-benzopyran-6-carbonitrile (1.50 g).

1. concentrationconcentrated under reduced pressure
2. dissolutionThe residue was dissolved in a mixture of ethyl acetate
3. washwashed with 5% hydrochloric acid (twice), aqueous sodium bicarbonate and brine
4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
5. customevaporated in vacuo
6. customThe residue was recrystallized from ethanol