Phosphorus oxychloride → HCID 13013934、化合物
反応式
O=[C:2]1[C:8]2[CH:9]=[CH:10][C:11]([C:13]([O:15][CH3:16])=[O:14])=[CH:12][C:7]=2[S:6](=[O:18])(=[O:17])[C:5]2[CH:19]=[CH:20][CH:21]=[CH:22][C:4]=2[NH:3]1.P(Cl)(Cl)(Cl)(Cl)[Cl:24].P(Cl)(Cl)(Cl)=O>>[Cl:24][C:2]1[C:8]2[CH:9]=[CH:10][C:11]([C:13]([O:15][CH3:16])=[O:14])=[CH:12][C:7]=2[S:6](=[O:18])(=[O:17])[C:5]2[CH:19]=[CH:20][CH:21]=[CH:22][C:4]=2[N:3]=1参加物
4
実験手順
Add 6.34 gm. (20 mmole) of finely powdered methyl 10,11-dihydro-11-oxodibenzo[b,f][1,4]thiazepin-3-carboxylate 5,5-dioxide to a mixture of 6.25 gm. (30 mmole) phosphorous pentachloride in 17.3 ml. of phosphoryl chloride. Stir for 18 hours at room temperature. Separate the solids by filtration, wash with ether and dry in vacuo over potassium hydroxide. Dissolve the crude product in boiling tetrahydrofuran, filter and evaporate to a small volume in a stream of nitrogen. Dilute with acetonitrile and separate the precipitate by filtration in order to obtain the title product. (m.p. 254°-256° C.).