Potassium Hydroxide → HCID 58495474, compound

Participants

Reaction Steps

Dissolve 3-(tert-butoxycarbonyl)-7-chloro-6-(4-dimethylcarbamoylthio-benzylamino)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (57 mg, 0.1 mmol) in methanol (5 mL). Add potassium hydroxide (65 mg, 1.1 mmol) and heat the mixture for 3 h at 65° C. Then add 1-bromo-3,3-dimethyl-2-butanone and heat at 65° C. for 2 h. Cool the mixture and dilute with EtOAc. Wash the organic phase with water, dry over MgSO4, filter and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/diethyl ether (7:3) to obtain the desired intermediate as an oil (18 mg, 30%).

Provenance & Evidence