Dichloromethane → HCID 13209440, Verbindung

HRID 620134

Reaktionsgleichung

Reaktionsgleichung von HRID 620134
[CH2:1]1[CH2:6][CH2:5][CH:4]([SH:7])[CH2:3][CH2:2]1.[C:8]1([N:14]2[C:19](=[O:20])[C:18]([Cl:21])=[C:17](Cl)[CH:16]=[N:15]2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(Cl)Cl.[OH-].[Na+]>[Cl-].C([N+](CC)(CC)CC1C=CC=CC=1)C.O>[C:8]1([N:14]2[C:19](=[O:20])[C:18]([Cl:21])=[C:17]([S:7][CH:4]3[CH2:5][CH2:6][CH2:1][CH2:2][CH2:3]3)[CH:16]=[N:15]2)[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

Komponenten

7

Edukt 4

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 15290CyclohexanethiolHCID 728134,5-Dichloro-2-phenyl-3(2H)-pyridazinone

Produkt 1

HCID 13209440HCID 13209440, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 66133Benzyl triethylammonium chlorideKatalysatorHCID 962WaterLösungsmittel

Versuchsvorschrift

38.3 parts by weight of cyclohexylthiol were added dropwise to a mixture of 72.3 parts by weight of 1-phenyl-4,5-dichloropyridazin-6-one in 300 parts by volume of methylene chloride, 3 parts by weight of triethylbenzylammonium chloride, and 13.2 parts by weight of sodium hydroxide in 150 parts by volume of water at room temperature (20° C.), and the reaction mixture was kept at this temperature for 12 hours, while stirring vigorously. The organic phase was separated off, washed with twice 100 parts by volume of water, dried and then concentrated. The residue was recrystallized from ethylacetate. 61 parts by weight of 1-phenyl-4-(cyclohexylthio)-5-chloropyridazin-6-one of melting point 125°-127° C. were obtained (compound A1).

Aufarbeitung

  1. customThe organic phase was separated off
  2. washwashed with twice 100 parts by volume of water
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was recrystallized from ethylacetate

Quellen und Nachweise

ORD-Eintrag
ord-387bee3514944a32aca67878a6c70e42
Quelldatensatz
uspto-grants-1989_04
Patentnummer
US04820704

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