反应详情

To a suspension of 3-ethyl-1,3,9,10,11,12-hexahydro-2H-quino[4,3,2-ef][1,4]benzoxazepin-2-one (5.0 g) in dry tetrahydrofuran (150 ml) was added potassium t-butoxide (3.0 g), with stirring. After 20 mins, methyl iodide (1.66 ml) was added, and the reaction mixture was stirred at room temperature overnight. The reaction mixture was concentrated, diluted with saturated potassium carbonate solution, and extracted with 2-butanone. The organic extracts were dried over anhydrous magnesium sulfate and concentrated. The residue was adhered to silica (methanol) and flash chromatographed (50% ethyl acetate/hexane). The appropriate fractions were concentrated and the residue was triturated with diethyl ether to give 3.59 g (68%) of 3-ethyl-1,3,9,10,11,12-hexahydro-1-methyl-2H-quino[4,3,2-ef][1,4]benzoxazepin-2-one.

1. stirringthe reaction mixture was stirred at room temperature overnight
2. concentrationThe reaction mixture was concentrated
3. additiondiluted with saturated potassium carbonate solution
4. extractionextracted with 2-butanone
5. dry with materialThe organic extracts were dried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. customchromatographed (50% ethyl acetate/hexane)
8. concentrationThe appropriate fractions were concentrated
9. customthe residue was triturated with diethyl ether