Methyl iodide → HCID 178461084, Verbindung

HRID 65948

Reaktionsgleichung

Reaktionsgleichung von HRID 65948
[CH2:1]([S:4]([NH2:7])(=O)=[O:5])[CH2:2][CH3:3].[OH-:8].[Na+].CI.[CH3:12]S(=NS(CCC)(=O)=O)C(=S)OC.C(S(N=SC(=S)O)(=O)=O)CC.[CH3:36][C:37]1[N:38]=[CH:39][NH:40][C:41]=1[CH2:42][S:43][CH2:44][CH2:45][NH2:46].[CH3:47][NH2:48]>C(O)C.CCCCCC.C(=S)=S>[CH3:47][NH:48][C:12]([NH:46][CH2:45][CH2:44][S:43][CH2:42][C:41]1[NH:40][CH:39]=[N:38][C:37]=1[CH3:36])=[N:7][S:4]([CH2:1][CH2:2][CH3:3])(=[O:5])=[O:8]

Komponenten

10

Edukt 7

HCID 6328Methyl iodideHCID 6329MethylamineHCID 14798Sodium HydroxideHCID 3401849Propane-1-sulphonamideHCID 86736200N-n-propanesulphonyliminodithiocarbonic acid dimethyl esterHCID 178433288HCID 178433288, VerbindungHCID 178461087HCID 178461087, Verbindung

Produkt 1

HCID 178461084HCID 178461084, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6348Carbon DisulfideLösungsmittelHCID 21879635Ethanol hexaneLösungsmittel

Versuchsvorschrift

Reaction of n-propanesulphonamide with sodium hydroxide, carbon disulphide and methyliodide by the method described in Example 8 afforded N-n-propanesulphonyliminodithiocarbonic acid dimethyl ester, m.p. 73°-74° (from ethanol-hexane). (Found: C, 31.7; H, 5.7; N, 6.2; S, 42.0. C6H13NO2S3 requires: C, 31.7; H, 5.8; N, 6.2; S, 42.3) (b) The reaction of N-n-propanesulphonyliminodithiocarbonic acid (4.7 g.) dimethyl ester with 4-methyl-5-((2-aminoethyl)thiomethyl)imidazole (3.5 g.) and methylamine by the method described in Example 7 followed by chromatographic purification on a column of silica gel with ethyl acetate-ethanol (4:1) as eluant afforded N-methyl-N'-[2-((4-methyl-5-imidazolyl)methylthio)ethyl]-N"-n-propanesulphonylguanidine as a glass (5.0 g.).

Aufarbeitung

  1. customfollowed by chromatographic purification on a column of silica gel with ethyl acetate-ethanol (4:1) as eluant

Quellen und Nachweise

ORD-Eintrag
ord-240baad454d847448efc3647cf438761
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04129657

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