1-Methylthio-1-methylamino-2-nitroethylene → Desmethylranitidine

HRID 127322

Reaktionsgleichung

Reaktionsgleichung von HRID 127322
[CH3:1][NH:2][CH2:3][C:4]1[O:8][C:7]([CH2:9][S:10][CH2:11][CH2:12][NH2:13])=[CH:6][CH:5]=1.[CH3:14][NH:15][C:16](SC)=[CH:17][N+:18]([O-:20])=[O:19]>>[CH3:1][NH:2][CH2:3][C:4]1[O:8][C:7]([CH2:9][S:10][CH2:11][CH2:12][NH:13][C:16]([NH:15][CH3:14])=[CH:17][N+:18]([O-:20])=[O:19])=[CH:6][CH:5]=1

Komponenten

3

Edukt 2

HCID 1235491-Methylthio-1-methylamino-2-nitroethyleneHCID 202094925-[[(2-Aminoethyl)thio]methyl]-N-methyl-2-furanmethanamine

Produkt 1

HCID 163116Desmethylranitidine

Versuchsvorschrift

A mixture of 2-[[[5-(methylamino)methyl-2-furanyl]methyl]thio]ethanamine (0.9 g) and N-methyl-1-methylthio-2-nitro-etheneamine was heated at 100°-120° for 30 mins under water pump pressure. The residue was purified by column chromatography (silica/methanol: 0.88 ammonia) to give N-[2-[[[5-(methylamino)methyl-2-furanyl]methyl]thio]ethyl]-N'-methyl-2-nitro-1,1-ethenediamine which was crystallised from acetonitrile m.p. 106°-108° (0.65 g).

Aufarbeitung

  1. temperaturewas heated at 100°-120° for 30 mins under water pump pressure
  2. customThe residue was purified by column chromatography (silica/methanol: 0.88 ammonia)

Quellen und Nachweise

ORD-Eintrag
ord-bcb94db76b4442c5b7791ef685e693ea
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04255440

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