反应详情

41 g. of 1-ethyl-5,6-dihydro-4-hydroxybenzo[5,6-cyclophepta[1,2-b]pyrazolo[4,3-e]pyridin-11(1H)-one (0.14 mol.) and 350 ml. of phosphorus oxychloride are refluxed for 4.5 hours. After cooling, the solution is filtered, the excess phosphorus oxychloride is removed in vacuo and the residue treated with water and extracted with chloroform. The chloroform extract is washed with water, dried with Na2SO4, treated with charcoal and then evaporated in vacuo to give 38 g. (87%) of 4-chloro-1-ethyl-5,6-dihydrobenzo[5,6]cyclohepta[1,2-b]pyrazolo[4,3-e]pyridin-11(1H)-one; m.p. 156°-159° (ethanol; refrigerator).

1. temperatureAfter cooling
2. filtrationthe solution is filtered
3. customthe excess phosphorus oxychloride is removed in vacuo
4. additionthe residue treated with water
5. extractionextracted with chloroform
6. extractionThe chloroform extract
7. washis washed with water
8. dry with materialdried with Na2SO4
9. additiontreated with charcoal
10. customevaporated in vacuo
11. customto give 38 g