Ammonia → Fenpiclonil

HRID 247104

Reaktionsgleichung

Reaktionsgleichung von HRID 247104
C([N:4]1[CH:8]=[C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([Cl:15])[C:10]=2[Cl:16])[C:6]([C:17](F)(F)F)=[CH:5]1)(=O)C.[NH3:21]>O1CCOCC1>[Cl:16][C:10]1[C:11]([Cl:15])=[CH:12][CH:13]=[CH:14][C:9]=1[C:7]1[C:6]([C:17]#[N:21])=[CH:5][NH:4][CH:8]=1

Komponenten

4

Edukt 2

HCID 222AmmoniaHCID 21245533N-Acetyl-4-(2,3-dichlorophenyl)-3-trifluoromethylpyrrole

Produkt 1

HCID 91724Fenpiclonil

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

6.4 g of N-acetyl-4-(2,3-dichlorophenyl)-3-trifluoromethylpyrrole, 15 ml of 25% aqueous ammonia solution and 60 ml of dioxane are stirred for 18 hours at 160° C. in an autoclave. The reaction mixture is cooled to room temperature and filtered, and the clear filtrate is concentrated by evaporation. The viscous residue is dissolved in ethyl acetate; the solution is washed firstly with water and then with a diluted sodium chloride solution; it is subsequently dried over sodium sulfate, filtered, and concentrated by evaporation. To the residue is added n-hexane, and the crystals which precipitate are filtered off and dried. The yield is 5.3 g of 4-(2,3-dichlorophenyl)-3-cyanopyrrole, m.p. 149°-150° C.

Aufarbeitung

  1. filtrationfiltered
  2. concentrationthe clear filtrate is concentrated by evaporation
  3. dissolutionThe viscous residue is dissolved in ethyl acetate
  4. washthe solution is washed firstly with water
  5. dry with materialit is subsequently dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated by evaporation
  8. additionTo the residue is added n-hexane
  9. filtrationthe crystals which precipitate are filtered off
  10. customdried

Quellen und Nachweise

ORD-Eintrag
ord-ebfe2d496bbb42d0a77e74f1a1e03a3d
Quelldatensatz
uspto-grants-1987_11
Patentnummer
US04705801

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