反应详情

To a solution of lithium aluminum hydride in tetrahydrofuran (1M, 14.8 ml) and dry tetrahydrofuran (30 ml) was added aluminum chloride (1.89 g) in portions, with stirring. After 5 mins, 3-ethyl-1,3,9,10,11,12-hexahydro-2H-quino[4,3,2-ef][1,4]benzoxazepin-2-one (4.0 g) was added, and the reaction mixture was stirred at room temperature overnight. Ethyl acetate (200 ml) and 10% sodium hydroxide solution (200 ml) were added. The organic phase was separated, dried over magnesium sulfate, filtered, and the filtrate was concentrated. The residue was flash chromatographed (5% triethylamine/toluene). The appropriate fractions were concentrated and treated with fumaric acid to give 4.05 g (74%) of product, mp 210° C.

1. stirringthe reaction mixture was stirred at room temperature overnight
2. customThe organic phase was separated
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. concentrationthe filtrate was concentrated
6. customchromatographed (5% triethylamine/toluene)
7. concentrationThe appropriate fractions were concentrated
8. additiontreated with fumaric acid