Water → HCID 22759921, compound

Participants

Reaction Steps

To a stirred suspension of 64.3 g (1.69 moles) of LiAlH4 in 1500 ml of anhydrous diethyl ether was added a solution of 144.0 g (0.537 mole) of crude 7-chloro-2,3-dihydro-5-phenyl-1,4-benzoxazepine produced in step (b) in 1000 ml of anhydrous diethyl ether, at a rate sufficient to maintain reflux. The mixture was initially blue, changing to a dark green which lightened with time. After addition was complete the mixture was stirred and refluxed for two hours. The reaction mixture was cooled and cautiously decomposed by the dropwise addition of 64.2 ml of water, followed by 64.2 ml of 15% NaOH solution and finally 192.6 ml of water. Stirring was continued for 30 minutes and then the inorganic solid was filtered off. The filter cake was washed well with diethyl ether and the combined filtrate and washings were dried over anhydrous Na2SO4.

Provenance & Evidence