Phosphorus oxychloride → HCID 178463015, Verbindung
Reaktionsgleichung
P(Cl)(Cl)(Cl)=[O:2].Cl[C:7]1[C:12]2[CH:13]=[N:14][N:15]([CH2:16][CH3:17])[C:11]=2[N:10]=[C:9]2[C:18](=[O:27])[C:19]3[CH:26]=[CH:25][CH:24]=[CH:23][C:20]=3[CH2:21][CH2:22][C:8]=12>C(O)C>[CH2:16]([N:15]1[C:11]2[N:10]=[C:9]3[C:18](=[O:27])[C:19]4[CH:26]=[CH:25][CH:24]=[CH:23][C:20]=4[CH2:21][CH2:22][C:8]3=[C:7]([OH:2])[C:12]=2[CH:13]=[N:14]1)[CH3:17]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
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).