Methylamine → 1-N'-[(6-chloropyridin-3-yl)methyl]-1-N-methyl-2-nitroethene-1,1-diamine

HRID 249508Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 249508
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][NH:9][C:10](SC)=[CH:11][N+:12]([O-:14])=[O:13])=[CH:4][CH:3]=1.[CH3:17][NH2:18]>CCO>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][NH:9][C:10]([NH:18][CH3:17])=[CH:11][N+:12]([O-:14])=[O:13])=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 6329MethylamineHCID 855929321-(6-Chloro-3-pyridylmethyl)amino-1-methylthio-2-nitroethylene

Produkt 1

HCID 43256191-N'-[(6-chloropyridin-3-yl)methyl]-1-N-methyl-2-nitroethene-1,1-diamineAusbeute 53,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

In 100 ml of EtOH was dissolved 1.2 g (4.6×10-3 mole) of 1-(6-chloro-3-pyridylmethyl)amino-1-methylthio-2-nitroethylene and on reflux, a solution of 0.84 g of 40% aqueous methylamine in 30 ml EtOH was added dropwise over 1 hour. After cooling, the reaction mixture was concentrated under reduced pressure to about 50 ml and the resulting crystals were collected by filtration and dried to give 0.6 g of the title compound as pale yellow needles.

Aufarbeitung

  1. temperatureon reflux
  2. temperatureAfter cooling
  3. concentrationthe reaction mixture was concentrated under reduced pressure to about 50 ml
  4. filtrationthe resulting crystals were collected by filtration
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-659fbe34b189419289ea8e87ff3e23ac
Quelldatensatz
uspto-grants-1993_05
Patentnummer
US05214152

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