Carbon Dioxide → HCID 86736244, compound

HRID 2163308Notes

Reaction equation

HRID 2163308 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[NH2:12][NH:13][C:14]([NH:16][NH2:17])=[O:15].C(=O)(O)[O-].[Na+].C(=O)=O>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:12][NH:13][C:14]([NH:16][NH2:17])=[O:15])(=[O:10])=[O:9])=[CH:4][CH:3]=1

Participants

6

Reactant 4

HCID 280Carbon Dioxide2×HCID 73984-Chlorobenzenesulfonyl chlorideHCID 73948CarbohydrazideHCID 516892Sodium Bicarbonate

Product 1

HCID 86736244HCID 86736244, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

211 (1.0 mole) p-chlorobenzenesulfonyl chloride was added to a suspension of 45 g (0.5 mole) carbohydrazide and 100 g sodium bicarbonate in 1000 ml ethanol in a 3 liter reaction flask. The mixture was stirred and heated gradually to gentle reflux (80° C) as carbon dioxide was evolved. Heating was continued until CO2 no longer evolved (3hours). The mix was cooled to 20 C and filtered. The mixture of product and sodium chloride was dried at 60° C. Yield = 227 g. The solid mixture was suspended in 2000 ml water, stirred to dissolve the sodium chloride, and then the insoluble product was filtered, washed and dried. Yield = 129 g, m.p. 239-240° C (dec.)

Workup

  1. temperatureheated gradually
  2. temperatureHeating
  3. custom(3hours)
  4. temperatureThe mix was cooled to 20 C
  5. filtrationfiltered
  6. additionThe mixture of product and sodium chloride
  7. customwas dried at 60° C
  8. stirringstirred
  9. dissolutionto dissolve the sodium chloride
  10. filtrationthe insoluble product was filtered
  11. washwashed
  12. customdried

Sources & evidence

ORD record
ord-8ca08687f7194a03a2837f75606430a2
Source dataset
uspto-grants-1979_01
Patent number
US04133832

Reaction notes

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