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Triethylamine → 4-[5-(3,5-Dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-methoxyphen yl trifluoromethane sulfonate

HRID 1844813
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1844813
[F:1][C:2]([F:19])([F:18])[S:3]([O:6][C:7]1[CH:12]=[CH:11][C:10]([CH:13]=[N:14][OH:15])=[CH:9][C:8]=1[O:16][CH3:17])(=[O:5])=[O:4].ClN1C(=O)CCC1=O.[Cl:28][C:29]1[CH:30]=[C:31]([C:36]([C:38]([F:41])([F:40])[F:39])=[CH2:37])[CH:32]=[C:33]([Cl:35])[CH:34]=1.C(N(CC)CC)C>CN(C)C=O>[F:19][C:2]([F:18])([F:1])[S:3]([O:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH2:37][C:36]([C:31]3[CH:32]=[C:33]([Cl:35])[CH:34]=[C:29]([Cl:28])[CH:30]=3)([C:38]([F:39])([F:41])[F:40])[O:15][N:14]=2)=[CH:9][C:8]=1[O:16][CH3:17])(=[O:4])=[O:5]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 8471TriethylamineHCID 31398ChlorosuccinimideHCID 231598231,3-Dichloro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzeneHCID 871503954-Hydroxyiminomethyl-2-methoxyphenyl trifluoromethane sulfonate

Produkt 1

HCID 231598024-[5-(3,5-Dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-methoxyphen yl trifluoromethane sulfonate
Ausbeute 41,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

In a solution of 2.0 g of 4-hydroxyiminomethyl-2-methoxyphenyl trifluoromethane sulfonate in 30 ml of N,N-dimethylformamide, 0.9 g of N-chlorosuccinic acid imide was added, and stirred at 40 to 50° C. for 30 minutes. Then, the reaction mixture was left and cooled to room temperature, 1.5 g of 3,5-dichloro-1-(1-trifluoromethylethenyl)benzene synthesized in Step 1 of Synthetic Example 3 and 0.7 g of triethylamine were added, and stirred at room temperature for 90 minutes. After the completion of the reaction, the reaction mixture was poured in 100 ml of ice water, extracted with ethyl acetate (50 ml×2), the organic phase was dehydrated with saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified with silica gel column chromatography that was eluated with ethyl acetate-hexane (1:7), and 1.4 g of the aimed product was obtained as colorless resinous substance.

Aufarbeitung

  1. waitThen, the reaction mixture was left
  2. temperaturecooled to room temperature
  3. stirringstirred at room temperature for 90 minutes
  4. customAfter the completion of the reaction
  5. extractionextracted with ethyl acetate (50 ml×2)
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off under reduced pressure
  8. customThe residue was purified with silica gel column chromatography that

Quellen und Nachweise

ORD-Eintrag
ord-5352fdef1ab44f5ab7c572fcfbd39983
Quelldatensatz
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08946492B2

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