Methyl Ethyl Ketone → HCID 178492798, Verbindung

HRID 22759

Reaktionsgleichung

Reaktionsgleichung von HRID 22759
Cl[C:2]1[N:3]=[N:4][C:5]([O:8][CH3:9])=[CH:6][CH:7]=1.NC(N)=[S:12].CC(CC)=O>O>[SH:12][C:2]1[N:3]=[N:4][C:5]([O:8][CH3:9])=[CH:6][CH:7]=1

Komponenten

5

Edukt 3

HCID 6569Methyl Ethyl KetoneHCID 744033-Chloro-6-methoxypyridazineHCID 2723790Thiourea

Produkt 1

HCID 178492798HCID 178492798, VerbindungAusbeute 24 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 3-chloro-6-methoxy pyridazine (0.69 mol, 100 g), thiourea (1.38 mol, 105 g) and ethyl methyl ketone (1.8 L) was refluxed for 3 hours. The reaction was cooled and the supernatant was poured into water and extracted with 1M sodium hydroxide (4×100 mL). The sodium hydroxide solution was washed with EtOAc (2×50 mL), the aqueous extract was acidified with sufficient conc. HCl to lower the pH to 5 and the resulting yellow solid was collected and air-dried to obtain 3-mercapto-6-methoxy pyridazine (24%, 23 g); mp 198° C.-200° C.

Aufarbeitung

  1. temperaturewas refluxed for 3 hours
  2. temperatureThe reaction was cooled
  3. extractionextracted with 1M sodium hydroxide (4×100 mL)
  4. washThe sodium hydroxide solution was washed with EtOAc (2×50 mL)
  5. extractionthe aqueous extract
  6. customthe resulting yellow solid was collected
  7. customair-dried

Quellen und Nachweise

ORD-Eintrag
ord-76473388b085410688169bdc886dcb6f
Quelldatensatz
uspto-grants-2005_02
Patentnummer
US06849629B2

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