反应详情

To a solution of 1-aminomethyl-7-methoxy-1,2,3,4-tetrahydro-1-naphthalenol (27.50 g) in 10% aqueous acetic acid solution (250 ml) was added dropwise a solution of sodium nitrite (10.07 g) in water (61 ml) at 8° C.~9° C. The reaction mixture was stirred for 2 hours at the same temperature. The resulting precipitates were collected by filtration. The precipitates were dissolved in ethyl acetate. The solution was dried over magnesium sulfate and evaporated in vacuo. The residue was purified by column chromatography (silica gel, n-hexane:ethyl acetate:chloroform=5:1:3) to give 3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-one (19.39 g) as a white powder.

1. customThe resulting precipitates
2. filtrationwere collected by filtration
3. dissolutionThe precipitates were dissolved in ethyl acetate
4. dry with materialThe solution was dried over magnesium sulfate
5. customevaporated in vacuo
6. customThe residue was purified by column chromatography (silica gel, n-hexane:ethyl acetate:chloroform=5:1:3)