Water → 2-(4-Chloro-2-fluoro-5-hydroxyphenyl)-4-methyl-5-(trifluoromethyl)-3(2H)-pyridazinone

HRID 1530788Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1530788
[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9]C(C)C)=[CH:4][C:3]=1[N:13]1[C:18](=[O:19])[C:17]([CH3:20])=[C:16]([C:21]([F:24])([F:23])[F:22])[CH:15]=[N:14]1.O>S(=O)(=O)(O)O>[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([OH:9])=[CH:4][C:3]=1[N:13]1[C:18](=[O:19])[C:17]([CH3:20])=[C:16]([C:21]([F:23])([F:24])[F:22])[CH:15]=[N:14]1

Komponenten

4

Edukt 2

HCID 962WaterHCID 110898282-(2-Fluoro-4-chloro-5-isopropoxyphenyl)-4-methyl-5-trifluoromethylpyridazin-3-one

Produkt 1

HCID 99490912-(4-Chloro-2-fluoro-5-hydroxyphenyl)-4-methyl-5-(trifluoromethyl)-3(2H)-pyridazinoneAusbeute 102,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

Then, 3.5 g (9.7 mmol) of 2-[2-fluoro-4-chloro-5-isopropoxyphenyl]-4-methyl-5-trifluoromethylpyridazin-3-one was dissolved in about 10 ml of concentrated sulfuric acid under ice cooling, and the solution was warmed to room temperature. After 10 minutes, about 100 ml of water was added to the reaction mixture. The precipitated crystals were collected by filtration and washed twice with 20 ml of water and then once with 10 ml of hexane. The resulting crystals were recrystallized from isopropanol to give 3.2 g (9.9 mmol) of 2-[2-fluoro-4-chloro-5-hydroxyphenyl]-4-methyl-5-trifluoromethylpyridazin-3-one.

Aufarbeitung

  1. filtrationThe precipitated crystals were collected by filtration
  2. washwashed twice with 20 ml of water
  3. customThe resulting crystals were recrystallized from isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-ef554a6b8ccc4859b03c0f93493fbc25
Quelldatensatz
uspto-grants-2001_03
Patentnummer
US06197727B1

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