Triethylamine → 2,6-Difluoro-N-(3-(3-(trifluoromethyl)phenyl)-5-isoxazolyl)benzamide

HRID 2059228

Reaktionsgleichung

Reaktionsgleichung von HRID 2059228
[F:1][C:2]([F:16])([F:15])[C:3]1[CH:4]=[C:5]([C:9]2[CH:13]=[C:12]([NH2:14])[O:11][N:10]=2)[CH:6]=[CH:7][CH:8]=1.C(N(CC)CC)C.[F:24][C:25]1[CH:33]=[CH:32][CH:31]=[C:30]([F:34])[C:26]=1[C:27](Cl)=[O:28]>C1C=CC=CC=1>[F:24][C:25]1[CH:33]=[CH:32][CH:31]=[C:30]([F:34])[C:26]=1[C:27]([NH:14][C:12]1[O:11][N:10]=[C:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:1])([F:15])[F:16])[CH:4]=2)[CH:13]=1)=[O:28]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 874382,6-Difluorobenzoyl chlorideHCID 130355443-(3-(Trifluoromethyl)phenyl)-1,2-oxazol-5-amine

Produkt 1

HCID 130355582,6-Difluoro-N-(3-(3-(trifluoromethyl)phenyl)-5-isoxazolyl)benzamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel2×

Versuchsvorschrift

3-(3-(Trifluoromethyl)phenyl)-5-aminoisoxazole (2.5 grams), triethylamine (1.5 grams) and 50 ml. benzene were placed in a 100 ml. flask. Next, 2,6-difluorobenzoylchloride (2.6 grams), dissolved in 5-10 ml. benzene, was added dropwise to the reaction mixture. The reaction was stirred at room temperature for 2 hours and was then warmed to 60° C. for about 18 hours. Following this, the mixture was washed with dilute sodium bicarbonate, water, brine, and then dried over MgSO4. The final product was first filtered, recrystallized from benzene/pentane, and then dried, m.p. 123°-126° C.

Aufarbeitung

  1. temperaturewas then warmed to 60° C. for about 18 hours
  2. washwas washed with dilute sodium bicarbonate, water, brine
  3. dry with materialdried over MgSO4
  4. customrecrystallized from benzene/pentane
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-166f8e1bc10d4d91888e4bbe0940cc85
Quelldatensatz
uspto-grants-1982_03
Patentnummer
US04322429

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