Hydrochloric Acid → HCID 178527979, Verbindung

HRID 1607583Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1607583
[NH2:1][NH:2][C:3]([NH2:5])=[S:4].[C:6](Cl)(=O)[C:7]1[CH:12]=[CH:11][CH:10]=[N:9][CH:8]=1.C(=O)([O-])[O-].[Na+].[Na+].Cl>N1C=CC=CC=1.O>[SH:4][C:3]1[N:5]=[C:6]([C:7]2[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=2)[NH:1][N:2]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 82604Nicotinoyl chlorideHCID 2723789Thiosemicarbazide

Produkt 1

HCID 178527979HCID 178527979, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 1049PyridineLösungsmittel

Versuchsvorschrift

To a solution of 19 g (0.200 mol) of thiosemicarbazide in 175 ml of dry pyridine, 29 g (0.200 mol) of nicotinoyl chloride was slowly added at 10° C. After reflux for 40 min. the reaction mixture was concentrated to half the original volume, 500 ml of water was added, and stored in the cold overnight. The precipitate formed was removed by filtration, and the filtrate was evaporated in vacuo. The resulting heavy, yellow oil was dissolved in 300 ml of water, and 64 g (0.600 mol) of sodium carbonate in 400 ml of water was added. After reflux for 4 h the solution was cooled and acidified with conc. hydrochloric acid to pH=4. The formed, colorless precipitate, 65, was isolated by filtration and dried in vacuo. Yield: 35 g (0.297 mol, 98%).

Aufarbeitung

  1. temperatureAfter reflux for 40 min. the reaction mixture
  2. concentrationwas concentrated to half the original volume, 500 ml of water
  3. additionwas added
  4. customstored in the cold overnight
  5. customThe precipitate formed
  6. customwas removed by filtration
  7. customthe filtrate was evaporated in vacuo
  8. dissolutionThe resulting heavy, yellow oil was dissolved in 300 ml of water
  9. temperatureAfter reflux for 4 h the solution
  10. temperaturewas cooled
  11. customThe formed, colorless precipitate, 65, was isolated by filtration
  12. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-c3b9aac5c3b74bbc88ccbdab0db592a4
Quelldatensatz
uspto-grants-1989_09
Patentnummer
US04866077

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