Sodium Chloride → HCID 85551694, compound

Participants

Reaction Conditions

Reaction Steps

5.36 g (22.5 m moles) of 2-phenyl-2,3,4,5-tetrahydro-1-benzoxepin-5-one (compound R1 of Reference Example 1) was dissolved in a mixture of 130 ml of tetrahydrofuran and 230 ml of ethyl ether, and 13.4 ml of hydrogen chloride-saturated ethyl ether was added to the solution, which was then cooled to -20° C. 5.79 ml (49.5 m moles) of sodium butylnitrite was added dropwise to the solution, and the reaction mixture was allowed to stand at -15° C. to -20° C. for two days. A saturated sodium chloride aqueous solution was added to the reaction mixture to separate the phases. An organic phase was obtained, washed with water, and dried with anhydrous magnesium sulfate. After filtrating off the magnesium sulfate, the filtrate was concentrated, and the concentrate was washed with hexane and dried to obtain 5.46 g (yield 90.8%) of the desired compound.

Provenance & Evidence