4-Toluenesulfonyl chloride → HCID 67620835, Verbindung

HRID 481312Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 481312
[CH2:1]([O:8][C:9]([C:11]1[CH:12]=[N+:13]([O-])[CH:14]=[CH:15][C:16]=1[CH3:17])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1(C)C=CC(S([Cl:28])(=O)=O)=CC=1>O1CCOCC1>[ClH:28].[CH2:1]([O:8][C:9]([C:11]1[CH:12]=[N:13][CH:14]=[CH:15][C:16]=1[CH2:17][Cl:28])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 73974-Toluenesulfonyl chlorideHCID 53818160HCID 53818160, Verbindung

Produkt 1

HCID 67620835HCID 67620835, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A mixture of the title compound of Preparation 7 (1.8 g, 7.3 mmol), p-toluenesulfonylchloride (2.0 g, 11 mmol) and dioxane (10 ml) was heated under reflux for 1.5 hours. The reaction mixutre was cooled to 0° C., diluted with water, treated with solid NaHCO3 and extracted with diethyl ether. The ether extracts were combined, dried (Na2 SO4), filtered and treated with HCl gas. The precipitate was filtered and washed with diethyl ether to afford 1.4 g of the title compound of this preparation. mp 149°-151° C. 1H NMR (CDCl3): δ 5.27 (2H, s), 5.42 (2H, s), 7.32-7.39 (5H, m), 8.35 (1H, d, J=6), 8.91 (1H, d, J=6), 9.28 (1H, s).

Quellen und Nachweise

ORD-Eintrag
ord-bd0ae2341e5c4d298a4fdb2a25dbb2fc
Quelldatensatz
uspto-grants-1998_08
Patentnummer
US05789408

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