Phosphorus oxychloride → HCID 13013934, Verbindung

Reaktionsgleichung

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

Komponenten

Edukt 3

HCID 24813Phosphorus oxychloride

HCID 24819Phosphorus pentachloride

HCID 13013925HCID 13013925, Verbindung

Produkt 1

HCID 13013934HCID 13013934, Verbindung

Versuchsvorschrift

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.).