反应详情

Phosphorus pentasulfide (5 mg, 0.01 mmol) was added to trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)formamide (5 mg, 0.015 mmol) in dioxane. The resulting mixture was heated to reflux for 3 h. After evaporation under reduced pressure the crude compound was chromatographed on silica. Elution with toluene/ethyl acetate 85:15 gave trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)methanethioamide (2.8 mg, 51%). Data: (m/z)=345 (M+H)+.

1. temperatureThe resulting mixture was heated
2. temperatureto reflux for 3 h
3. customAfter evaporation under reduced pressure the crude compound
4. customwas chromatographed on silica
5. washElution with toluene/ethyl acetate 85:15