Sodium hydrosulfide → 2-t-butyl-5-mercapto-4-methyl-3(2H)-pyridazinone

HRID 2352013Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2352013
[C:1]([N:5]1[C:10](=[O:11])[C:9]([CH3:12])=[C:8](Cl)[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].[SH-:14].[Na+]>C(O)C>[C:1]([N:5]1[C:10](=[O:11])[C:9]([CH3:12])=[C:8]([SH:14])[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2]

Komponenten

4

Edukt 2

HCID 28015Sodium hydrosulfideHCID 138222642-tert-butyl-5-chloro-4-methylpyridazin-3-(2H)-one

Produkt 1

HCID 138222652-t-butyl-5-mercapto-4-methyl-3(2H)-pyridazinoneAusbeute 96,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To 75ml of ethanol were added 17.0 g (0.085 mol) of 2-tert.-butyl-5-chloro-4-methyl-3(2H)-pyridazinone and 8.5 g (0.106 mol) of 70% sodium hydrosulfide, and the mixture was stirred under reflux for 4 hours. After cooling, the mixture was poured into 300 ml of ice-water and extracted with 200 ml of ethyl ether. The ether layer was washed with 100 ml of water and dried over anhydrous sodium sulfate. The solvent was then distilled off therefrom to give 16.3 g of a crude product.

Aufarbeitung

  1. temperatureunder reflux for 4 hours
  2. temperatureAfter cooling
  3. extractionextracted with 200 ml of ethyl ether
  4. washThe ether layer was washed with 100 ml of water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent was then distilled off

Quellen und Nachweise

ORD-Eintrag
ord-ea6e550985fa4ef7a3b733fbe95e7ea3
Quelldatensatz
uspto-grants-1989_10
Patentnummer
US04874861

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