Phosphorus oxychloride → 3-Chloro-6-[3-(trifluoromethyl)phenyl]pyridazine

HRID 372730

Reaktionsgleichung

Reaktionsgleichung von HRID 372730
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]2[CH:10]=[CH:11][C:12](=O)[NH:13][N:14]=2)[CH:4]=1.P(Cl)(Cl)([Cl:20])=O>>[F:1][C:2]([F:17])([F:16])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]2[N:14]=[N:13][C:12]([Cl:20])=[CH:11][CH:10]=2)[CH:4]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 124495416-[3-(Trifluoromethyl)phenyl]pyridazin-3-ol

Produkt 1

HCID 124495523-Chloro-6-[3-(trifluoromethyl)phenyl]pyridazine

Versuchsvorschrift

A mixture of 12.6 g. of 6-(α,α,α-trifluoro-m-tolyl)-3(2H)-pyridazinone and 200 ml. of phosphorus oxychloride is heated on a steam bath for 18 hours. The mixture is concentrated under vacuum and the residue triturated with cold water. The resulting solid is washed with water and air dried to give 13.5 g. of cream colored crystals, m.p. 131°-133° C. Recrystallization from methanol gives 6-(α,α,α-trifluoro-m-tolyl)-3-chloropyridazine as white crystals, m.p. 131°-133° C.

Aufarbeitung

  1. additionA mixture of 12.6 g
  2. concentrationThe mixture is concentrated under vacuum
  3. customthe residue triturated with cold water
  4. washThe resulting solid is washed with water and air
  5. customdried
  6. customto give 13.5 g
  7. customRecrystallization from methanol

Quellen und Nachweise

ORD-Eintrag
ord-de7977de5bee49989108fd2055ef3762
Quelldatensatz
uspto-grants-1978_05
Patentnummer
US04092311

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