反应详情

30.0 G. of dibenzo[b,e]thiepin-11(6H)-one are heated to 180° C. with 300 ml. of 3-amino-1-propanol. The water formed and the excess amine are distilled off for 2 hours and the residue is then cooled, diluted with methylene chloride and washed several times with distilled water. The organic phase is dried over sodium sulfate and evaporated. After chromatographic purification over silica gel using toluene for the elution, there is obtained 3-{(dibenzo[b,e]-thiepin-11(6H)-yliden)-amino}-1-propanol.

1. distillationthe excess amine are distilled off for 2 hours
2. temperaturethe residue is then cooled
3. additiondiluted with methylene chloride
4. washwashed several times with distilled water
5. dry with materialThe organic phase is dried over sodium sulfate
6. customevaporated
7. customAfter chromatographic purification over silica gel
8. washfor the elution