反应详情

To a solution of lithium aluminum hydride in tetrahydrofuran (1M, 11.99 ml) and dry tetrahydrofuran (30 ml) was added aluminum chloride (1.6 g) in portions, with stirring. After five mins, 3-ethyl-1,3,9,10,11,12-hexahydro-1-methyl-2H-quino[4,3,2-ef][1,4]benzoxazepin-2-one (3.55 g) was added, and stirring was continued for 0.5 hr. Ethyl acetate (200 ml) and 10% sodium hydroxide solution (200 ml) were added, the organic layer was separated, dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated. The residue was flash chromatographed (1.5% triethylamine/toluene). The appropriate fractions were concentrated and the residue was treated with fumaric acid followed by recrystallization from methanol to give 1.82 g (38%) of product, mp 243° C. (dec.).

1. stirringstirring
2. waitwas continued for 0.5 hr
3. customthe organic layer was separated
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. concentrationthe filtrate was concentrated
7. customchromatographed (1.5% triethylamine/toluene)
8. concentrationThe appropriate fractions were concentrated
9. additionthe residue was treated with fumaric acid
10. customfollowed by recrystallization from methanol