Diethyl Ether → HCID 12338798, compound

Participants

Reaction Steps

To a suspension of 20 parts of 1-(10-bromo-5H-dibenzo[a,d]cyclohepten-5-yl)-4-nitrosopiperazine in 1400 parts of anhydrous ether is slowly added 7 parts of lithium tetrahydroaluminate(1-). The resultant mixture is stirred at room temperatures for 5 hours, then cooled to around 5° and maintained thereat while a solution of 14 parts of water in 25 parts of tetrahydrofuran, 18 parts of aqueous 25% sodium hydroxide, and 14 parts of water are consecutively introduced. Insoluble solids are removed by filtration and washed with tetrahydrofuran. The washings and filtrate are combined, dried over anhydrous magnesium sulfate, and stripped of solvent by vacuum distillation. The residual yellow solid is crystallized from a mixture of tetrahydrofuran and hexane to give 1-(10-bromo-5H-dibenzo[a,d]cyclohepten-5-yl)-4-piperazineamine as colorless crystals melting at 187.5°-190.5°.

Provenance & Evidence