Methylhydrazine → HCID 178498595, Verbindung

HRID 362652

Reaktionsgleichung

Reaktionsgleichung von HRID 362652
[C:1]([C:7]([O:9][CH3:10])=[O:8])#[C:2][C:3](OC)=[O:4].[CH3:11][NH:12][NH2:13]>CCOCC>[OH:4][C:3]1[N:12]([CH3:11])[N:13]=[C:1]([C:7]([O:9][CH3:10])=[O:8])[CH:2]=1

Komponenten

4

Edukt 2

HCID 6061MethylhydrazineHCID 12980Dimethyl acetylenedicarboxylate

Produkt 1

HCID 178498595HCID 178498595, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Reaktionsbedingungen

Temperatur
-5 °C

Versuchsvorschrift

102.3 g (0.72 mol) Dimethyl acetylenedicarboxylate was added to 1000 ml ether and the mixture cooled to -5° C. in an ice-methanol bath. 33 g (0.72 mol) methylhydrazine in 100 ml ether was added dropwise at a rate that the inner temperature did not rise above 0° C. The mixture was stirred for one hour at 0° C., the precipitate suction filtered off, washed with ether and dried at 40° C. in vacuo. The intermediate was immersed in an oil-bath heated to 120° C. The reaction product was recrystallised from methanol.

Aufarbeitung

  1. customdid not rise above 0° C
  2. filtrationthe precipitate suction filtered off
  3. washwashed with ether
  4. customdried at 40° C. in vacuo
  5. customThe intermediate was immersed in an oil-bath
  6. temperatureheated to 120° C
  7. customThe reaction product was recrystallised from methanol

Quellen und Nachweise

ORD-Eintrag
ord-c57b0a82a8434593bae231040cfa0921
Quelldatensatz
uspto-grants-1999_02
Patentnummer
US05869686

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