Carbon Dioxide → 1,5-Bis(p-toluene sulfonyl) carbohydrazide

HRID 839478Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 839478
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7](Cl)(=[O:9])=[O:8])=[CH:3][CH:2]=1.[NH2:12][NH:13][C:14]([NH:16][NH2:17])=[O:15].C(=O)(O)[O-].[Na+].C(=O)=O>CO>[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7]([NH:12][NH:13][C:14]([NH:16][NH:17][S:7]([C:4]2[CH:5]=[CH:6][C:1]([CH3:11])=[CH:2][CH:3]=2)(=[O:9])=[O:8])=[O:15])(=[O:9])=[O:8])=[CH:3][CH:2]=1

Komponenten

6

Edukt 4

HCID 280Carbon DioxideHCID 73974-Toluenesulfonyl chlorideHCID 73948CarbohydrazideHCID 516892Sodium Bicarbonate

Produkt 1

HCID 2279791,5-Bis(p-toluene sulfonyl) carbohydrazide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

190.5 g (1.0 mole) p-toluene sulfonyl chloride, 45 g (0.5 mole) carbohydrazide, 84 g (1.0 mole) sodium bicarbonate and 1000 ml methanol were placed in a 2 liter flask. The mixture was stirred and heated to reflux (65° C) for 90 minutes. Carbon dioxide evolution was complete at this point. The solid product and sodium chloride were filtered off. The material was suspended in water to dissolve the sodium chloride and the residual solid product was filtered off, washed well with water, and dried at 60° C. Yield: 139 g -- Dec. temp. 232° C.

Aufarbeitung

  1. temperatureheated
  2. filtrationThe solid product and sodium chloride were filtered off
  3. dissolutionto dissolve the sodium chloride
  4. filtrationthe residual solid product was filtered off
  5. washwashed well with water
  6. customdried at 60° C

Quellen und Nachweise

ORD-Eintrag
ord-549acd249abf4ece84008905ee97e360
Quelldatensatz
uspto-grants-1978_06
Patentnummer
US04096100

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