Oxalic acid dihydrate → N,N-dimethyl-3-[3-[(1-methylthio-2-nitroethenyl)amino]propoxy]benzenemethanamine

HRID 1659572Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1659572
[NH2:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]([CH2:12][N:13]([CH3:15])[CH3:14])[CH:9]=[CH:10][CH:11]=1.[CH3:16][S:17][CH:18](SC)[CH2:19][N+:20]([O-:22])=[O:21].O.O.C(O)(=O)C(O)=O>O1CCCC1>[CH3:15][N:13]([CH3:14])[CH2:12][C:8]1[CH:9]=[CH:10][CH:11]=[C:6]([O:5][CH2:4][CH2:3][CH2:2][NH:1][C:18]([S:17][CH3:16])=[CH:19][N+:20]([O-:22])=[O:21])[CH:7]=1

Komponenten

5

Edukt 3

HCID 61373Oxalic acid dihydrateHCID 123722641,1-Bis(methylsulfanyl)-2-nitroethaneHCID 129139503-(3-Aminopropoxy)-N,N-dimethylbenzenemethanamine

Produkt 1

HCID 70538402N,N-dimethyl-3-[3-[(1-methylthio-2-nitroethenyl)amino]propoxy]benzenemethanamineAusbeute 64 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

3-(3-Aminopropoxy)-N,N-dimethylbenzenemethanamine (10 g) and 1,1-bis-(methylthio)-2-nitroethane (16 g) were heated under reflux in tetrahydrofuran for 19 hours. Oxalic acid dihydrate (1.3 g) was added and the resulting precipitate was discarded. The solvent was removed to leave the title compound as a crystalline solid (10 g) m.p. 59°-63°.

Aufarbeitung

  1. customThe solvent was removed

Quellen und Nachweise

ORD-Eintrag
ord-1baaf465976a43f6b352682f54b4b04b
Quelldatensatz
uspto-grants-1981_12
Patentnummer
US04304780

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