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Hydrazine hydrate (1:1) → HCID 67356224, Verbindung

HRID 405705
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 405705
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([C:34]([F:37])([F:36])[F:35])[O:13][N:12]([CH3:14])[C:11]([C:15]3[CH:32]=[CH:31][C:18]([CH2:19][N:20]4C(=O)C5C(=CC=CC=5)C4=O)=[C:17]([CH3:33])[CH:16]=3)=[CH:10]2)[CH:5]=[C:6]([Cl:8])[CH:7]=1.O.NN>C(O)C.C(OCC)C>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([C:34]([F:36])([F:35])[F:37])[O:13][N:12]([CH3:14])[C:11]([C:15]3[CH:32]=[CH:31][C:18]([CH2:19][NH2:20])=[C:17]([CH3:33])[CH:16]=3)=[CH:10]2)[CH:5]=[C:6]([Cl:8])[CH:7]=1
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Komponenten

5

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 533715112-{4-[5-(3,5-Dichloro-phenyl)-2-methyl-5-trifluoromethyl-2,5-dihydro-isoxazol-3-yl]-2-methyl-benzyl}-isoindole-1,3-dione

Produkt 1

HCID 67356224HCID 67356224, VerbindungAusbeute 65 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 3283
Diethyl Ether
Lösungsmittel

Versuchsvorschrift

837 mg of 2-{4-[5-(3,5-Dichloro-phenyl)-2-methyl-5-trifluoromethyl-2,5-dihydro-isoxazol-3-yl]-2-methyl-benzyl}-isoindole-1,3-dione (Example I14) and 500 mg hydrazine hydrate in 25 ml ethanol were heated at reflux for 2 hours under stirring. The mixture was cooled and diluted with diethyl ether. The solid was filtered off and the filtrate was evaporated. The residue was dissolved in 100 ml of ether and washed with water. The organic phase was dried and evaporated. The residue was purified on silica gel (eluent dichloromethane/methanol 4:1) affording 4-[5-(3,5-dichloro-phenyl)-2-methyl-5-trifluoromethyl-2,5-dihydro-isoxazol-3-yl]-2-methyl-benzylamine as a resin in 65% yield. 1H-NMR (CDCl3, δ in ppm): 7.44 (s, 2H), 7.37 (m, 2H), 7.28 (m, 2H), 5.33 (s, 1H), 3.88 (s, 2H), 2.99 (s, 3H), 2.34 (s, 3H).

Aufarbeitung

  1. temperatureat reflux for 2 hours
  2. temperatureThe mixture was cooled
  3. filtrationThe solid was filtered off
  4. customthe filtrate was evaporated
  5. dissolutionThe residue was dissolved in 100 ml of ether
  6. washwashed with water
  7. customThe organic phase was dried
  8. customevaporated
  9. customThe residue was purified on silica gel (eluent dichloromethane/methanol 4:1)

Quellen und Nachweise

ORD-Eintrag
ord-a9eaee1ed88c4f3f825471820d9b03d6
Quelldatensatz
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08754053B2

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