Dimethylformamide dimethyl acetal → 4-[5-(3,5-Dichlorophenyl)-5-(trifluoromethyl)-4,5-dihydroisoxazole-3-yl]-N-[(dimethylamino)methylene]-2-methylbenzamide

HRID 1187980Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1187980
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([C:24]([F:27])([F:26])[F:25])[O:13][N:12]=[C:11]([C:14]3[CH:22]=[CH:21][C:17]([C:18]([NH2:20])=[O:19])=[C:16]([CH3:23])[CH:15]=3)[CH2:10]2)[CH:5]=[C:6]([Cl:8])[CH:7]=1.CO[CH:30](OC)[N:31]([CH3:33])[CH3:32]>>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([C:24]([F:25])([F:27])[F:26])[O:13][N:12]=[C:11]([C:14]3[CH:22]=[CH:21][C:17]([C:18]([N:20]=[CH:30][N:31]([CH3:33])[CH3:32])=[O:19])=[C:16]([CH3:23])[CH:15]=3)[CH2:10]2)[CH:5]=[C:6]([Cl:8])[CH:7]=1

Komponenten

3

Edukt 2

HCID 78373Dimethylformamide dimethyl acetalHCID 667845734-(5-(3,5-Dichlorophenyl)-5-(trifluoromethyl)-4,5-dihydroisoxazol-3-yl)-2-methylbenzamide

Produkt 1

HCID 547675024-[5-(3,5-Dichlorophenyl)-5-(trifluoromethyl)-4,5-dihydroisoxazole-3-yl]-N-[(dimethylamino)methylene]-2-methylbenzamide

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A mixture of 6.0 g of 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole-3-yl]-2-methyl benzoic acid amide synthesized in Step 1 of Synthetic Example 19 and 50 mL of N,N-dimethylformamide dimethylacetal were stirred at 120° C. for 1.5 hour. After the completion of the reaction, the solvent was distilled off under reduced pressure. The residual solid was washed with ethyl acetate-hexane mixture (1:20) to obtain 6.2 g of the aimed product as pale yellow crystal.

Aufarbeitung

  1. customAfter the completion of the reaction
  2. distillationthe solvent was distilled off under reduced pressure
  3. washThe residual solid was washed with ethyl acetate-hexane mixture (1:20)

Quellen und Nachweise

ORD-Eintrag
ord-ed70697296064a129e494214c7663224
Quelldatensatz
uspto-grants-2014_03
Patentnummer
US08673951B2

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