Acetic Acid → 3-[3-(6-Methoxy-m-tolyl)-1,2-benzisoxazol-5-yl]-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione

HRID 369585Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 369585
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][N:8]=[C:7]([C:10]3[CH:11]=[C:12]([CH3:18])[C:13]([O:16][CH3:17])=[CH:14][CH:15]=3)[C:6]=2[CH:19]=1.CN(C)[C:22]1[O:23][C:24](=[O:32])[CH:25]=[C:26]([C:28]([F:31])([F:30])[F:29])[N:27]=1.C(O)(=O)C>O>[CH3:17][O:16][C:13]1[C:12]([CH3:18])=[CH:11][C:10]([C:7]2[C:6]3[CH:19]=[C:2]([N:1]4[C:24](=[O:32])[CH:25]=[C:26]([C:28]([F:31])([F:30])[F:29])[NH:27][C:22]4=[O:23])[CH:3]=[CH:4][C:5]=3[O:9][N:8]=2)=[CH:15][CH:14]=1

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 37238622-(dimethylamino)-4-(trifluoromethyl)-6H-1,3-oxazin-6-oneHCID 698321145-Amino-3-(6-methoxy-m-tolyl)-1,2-benzisoxazole

Produkt 1

HCID 700979223-[3-(6-Methoxy-m-tolyl)-1,2-benzisoxazol-5-yl]-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 5-amino-3-(6-methoxy-m-tolyl)-1,2-benzisoxazole (8.40 g, 0.033 mol), 2-dimethylamino-4-(trifluoromethyl)-6H-1,3-oxazin-6-one (7.60 g, 0.036 mol), and acetic acid is refluxed for three hours, cooled, poured onto ice, and diluted with water. The resultant aqueous mixture is filtered to obtain a solid. The solid is washed with water and dried to give the title product as a pink solid which is identified by NMR spectral analyses.

Aufarbeitung

  1. temperatureis refluxed for three hours
  2. temperaturecooled
  3. additionpoured onto ice
  4. filtrationThe resultant aqueous mixture is filtered
  5. customto obtain a solid
  6. washThe solid is washed with water
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-a1f22c61211c472192de931e37377717
Quelldatensatz
uspto-grants-2000_10
Patentnummer
US06140270

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