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Ethanol → 1-(2,6-Dichloro-4-trifluoromethylphenyl)-5-(pyrazin-2-ylmethylamino)pyrazole-3-carbonitrile

HRID 22865
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 22865
C(O)C.[BH4-].[Na+].[Cl:6][C:7]1[CH:12]=[C:11]([C:13]([F:16])([F:15])[F:14])[CH:10]=[C:9]([Cl:17])[C:8]=1[N:18]1[C:22](=[N:23][CH:24]([C:26]2[CH:31]=[N:30][CH:29]=[CH:28][N:27]=2)Cl)[CH:21]=[C:20]([C:32]#[N:33])[NH:19]1.O>C(OCC)(=O)C>[Cl:17][C:9]1[CH:10]=[C:11]([C:13]([F:14])([F:15])[F:16])[CH:12]=[C:7]([Cl:6])[C:8]=1[N:18]1[C:22]([NH:23][CH2:24][C:26]2[CH:31]=[N:30][CH:29]=[CH:28][N:27]=2)=[CH:21][C:20]([C:32]#[N:33])=[N:19]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 702EthanolHCID 962WaterHCID 4311764Sodium borohydrideHCID 178510205HCID 178510205, Verbindung

Produkt 1

HCID 112007821-(2,6-Dichloro-4-trifluoromethylphenyl)-5-(pyrazin-2-ylmethylamino)pyrazole-3-carbonitrileAusbeute 92,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857
Ethyl Acetate
Lösungsmittel

Versuchsvorschrift

To an ethanol (2 ml) suspension of 85 mg (2.2 mmol) of sodium borohydride was gradually added 0.5 g (1.1 mmol) of 1-(2,6-dichloro-4-trifluoromethylphenyl)-5-(pyrazin-2-ylchloromethylimino)pyrazole-3-carbonitrile at 20° C. or less. After 1 hour of stirring at room temperature, the mixture was gradually poured into 40 ml of water to precipitate crystals. After 30 minutes of stirring, the crystals were filtrated and washed with water until the pH of the filtrate became 6. The crystals thus obtained were dissolved in ethyl acetate and the solution was extracted after the addition of saturated saline. The organic layer was dried over anhydrous magnesium sulfate, filtrated, and concentrated. The resulting crystals were filtrated, washed with a small amount of hexane and ethyl acetate, and dried to obtain 0.42 g (yield 92%) of 1-(2,6-dichloro-4-trifluoromethylphenyl)-5-(pyrazin-2-ylmethylamino)pyrazole-3-carbonitrile.

Aufarbeitung

  1. customat 20° C. or less
  2. customto precipitate crystals
  3. stirringAfter 30 minutes of stirring
  4. filtrationthe crystals were filtrated
  5. washwashed with water until the pH of the filtrate
  6. customThe crystals thus obtained
  7. extractionthe solution was extracted
  8. additionafter the addition of saturated saline
  9. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  10. filtrationfiltrated
  11. concentrationconcentrated
  12. filtrationThe resulting crystals were filtrated
  13. washwashed with a small amount of hexane and ethyl acetate
  14. customdried

Quellen und Nachweise

ORD-Eintrag
ord-db2bf85eb63c4acfa9854fc007a96251
Quelldatensatz
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06849633B2

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