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Ammonia → HCID 13561854, Verbindung

HRID 622283
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 622283
[C:1](Cl)(=[O:4])[CH2:2][CH3:3].[NH2:6][C:7]1[N:11]([C:12]2[CH:17]=[CH:16][C:15]([O:18][C:19]([F:22])([F:21])[F:20])=[CH:14][C:13]=2[Cl:23])[N:10]=[CH:9][C:8]=1[C:24]#[N:25].N1C=CC=CC=1.N>C(Cl)(Cl)Cl.C(O)C>[C:24]([C:8]1[CH:9]=[N:10][N:11]([C:12]2[CH:17]=[CH:16][C:15]([O:18][C:19]([F:21])([F:22])[F:20])=[CH:14][C:13]=2[Cl:23])[C:7]=1[NH:6][C:1](=[O:4])[CH2:2][CH3:3])#[N:25]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 222AmmoniaHCID 1049PyridineHCID 62324Propionyl chlorideHCID 135618335-Amino-4-cyano-1-(2-chloro-4-trifluoromethoxy-phenyl)-pyrazole

Produkt 1

HCID 13561854HCID 13561854, VerbindungAusbeute 75,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702
Ethanol
Lösungsmittel
HCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

10 ml (0.11 mole) of propionyl chloride are added to 2.9 g (0.01 mole) of 5-amino-4-cyano-1-(2-chloro-4-trifluoromethoxy-phenyl)-pyrazole in 30 ml of chloroform at 0° C., with stirring, and a solution of 1.8 ml (0.02 mole) of pyridine in 15 ml of chloroform is then added, also at 0° C. When the addition has ended, stirring is continued at room temperature for 20 hours, the solvent is stripped off, the residue is taken up in 50 ml of ethanol, aqueous ammonia is added until the reaction is alkaline, the volatile constitutents are removed in vacuo, the residue is taken up in 100 ml of chloroform, the mixture is washed with water, then with 2N hydrochloric acid and again with water and dried over sodium sulphate and the solvent is removed in vacuo. 2.7 g (75.3% of theory) of 4-cyano-1-(2-chloro-4-trifluoromethoxy-phenyl)-5-propionylamino-pyrazole of melting point 127° C. are obtained.

Aufarbeitung

  1. additionWhen the addition
  2. stirringstirring
  3. customthe volatile constitutents are removed in vacuo
  4. washthe mixture is washed with water
  5. dry with materialwith 2N hydrochloric acid and again with water and dried over sodium sulphate
  6. customthe solvent is removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-48cca334ef2f44d3b07188eafbb89f42
Quelldatensatz
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04770693

Notizen zur Reaktion

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