Ethyl Acetate → HCID 68642115, compound

Participants

Reaction Steps

Lithium aluminum hydride (76 mg, 2.00 mmol) was suspended in tetrahydrofuran (20 ml), and under an ice cooling, a solution (10 ml) of ethyl 3,4-dihydro-1H-2-thia-4a,9-diazafluorene-7-carboxylate (260 mg, 1.00 mmol) prepared in the Step 40-1-3 in tetrahydrofuran was slowly added to the suspension. After the mixture was stirred under an ice cooling for 30 minutes, under an ice cooling, a saturated sodium bicarbonate solution was slowly added to the mixture, and then ethyl acetate was added thereto. The resulting mixture was filtered, and the residue was washed with a mixture solution of chloroform and methanol. The filtrate was concentrated and purified by silica gel column chromatography (chloroform:methanol=50:1) to give the title compound (150 mg, 68%) as a white powder.

Provenance & Evidence