Phosgene → Cyclohexylsulfamyl chloride

HRID 866772

Reaktionsgleichung

Reaktionsgleichung von HRID 866772
[Cl-].[Cl:2]C(=[N+](C)C)Cl.C(Cl)(Cl)=O.[CH:12]1([NH:18][S:19](=[O:22])(=O)[OH:20])[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1>ClCCCl>[CH:12]1([NH:18][S:19]([Cl:2])(=[O:22])=[O:20])[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1

Komponenten

5

Edukt 3

HCID 6371Phosgene2×HCID 7533CyclamateHCID 2723945Phosgeniminium chloride

Produkt 1

HCID 12914615Cyclohexylsulfamyl chlorideAusbeute 68 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 111,2-DichloroethaneLösungsmittel

Versuchsvorschrift

15 parts of dichloromethylenedimethylammonium chloride, suspended in 540 parts of 1,2-dichloroethane, are saturated with 40 parts of phosgene at 35° C, whilst stirring. 89.6 parts of cyclohexylsulfamic acid are now added and a further 550 parts of phosgene are then introduced in the course of 15 hours at 83° C, whilst stirring. After removing excess phosgene, and the solvent, under reduced pressure, 67.2 parts (68% of theory) of cyclohexylsulfamic acid chloride of boiling point 100°-114° C/0.01 mm Hg and melting point 43°-47° C are obtained by distillation of the residue.

Aufarbeitung

  1. stirringwhilst stirring
  2. customAfter removing excess phosgene

Quellen und Nachweise

ORD-Eintrag
ord-446bc1bbaa5e4c3fb941c130704c3038
Quelldatensatz
uspto-grants-1978_07
Patentnummer
US04101571

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