Acetone → N-Methyl-1-(methylsulfanyl)-2-nitroethan-1-amine

HRID 65757

Reaktionsgleichung

Reaktionsgleichung von HRID 65757
CNCC1OC(CSCCN)=CC=1.[CH3:14][NH:15][C:16]([S:21][CH3:22])=[CH:17][N+:18]([O-:20])=[O:19].CC(C)=O>O>[CH3:14][NH:15][CH:16]([S:21][CH3:22])[CH2:17][N+:18]([O-:20])=[O:19]

Komponenten

5

Edukt 3

HCID 180AcetoneHCID 1235491-Methylthio-1-methylamino-2-nitroethyleneHCID 202094925-[[(2-Aminoethyl)thio]methyl]-N-methyl-2-furanmethanamine

Produkt 1

HCID 15788612N-Methyl-1-(methylsulfanyl)-2-nitroethan-1-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 2-[[[5-(methylamino)methyl-2-furanyl]methyl]thio]ethanamine (10 g, 0.05 mole) and N-methyl-1-methylthio-2-nitroetheneamine (7.4 g) in water (25 ml) was stirred at 50° for 2 hr. Acetone (350 ml) was added and the solvent was removed by distillation at atmospheric pressure until 275 ml of distillate had been collected. Ethanolic hydrogen chloride (2M; 27.5 ml) was added to the residue and the solution was stirred overnight at room temperature. The product (11.0 g) m.p. 161°, was collected and recrystallised from ethanol as a colourless microcrystalline solid (10.1 g) m.p. 162°. Analysis Found: C, 42.6; H, 6.3; N, 16.4. C12H20N4O3S.HCl requires: C, 42.8; H, 6.2; N, 16.6%.

Aufarbeitung

  1. customthe solvent was removed by distillation at atmospheric pressure until 275 ml of distillate
  2. customhad been collected
  3. additionEthanolic hydrogen chloride (2M; 27.5 ml) was added to the residue
  4. customThe product (11.0 g) m.p. 161°, was collected
  5. customrecrystallised from ethanol as a colourless microcrystalline solid (10.1 g) m.p. 162°

Quellen und Nachweise

ORD-Eintrag
ord-879e2c1022f9429e8dc3684aeda99831
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04128658

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