Potassium Dichromate → HCID 11187860, Verbindung

HRID 48984

Reaktionsgleichung

Reaktionsgleichung von HRID 48984
[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=O.[K+].[K+].[OH:12][CH2:13][C:14]1[C:18]2[CH:19]=[C:20]([N:23]3[C:28](=[O:29])[CH:27]=[C:26]([C:30]([F:33])([F:32])[F:31])[N:25]([CH3:34])[C:24]3=[O:35])[CH:21]=[CH:22][C:17]=2[S:16][N:15]=1.CN1C(C(F)(F)F)=CC(=[O:47])N(C2C=CC3SN=C(C=O)C=3C=2)C1=O>S(=O)(=O)(O)O.C(O)(=O)C.O>[CH3:34][N:25]1[C:26]([C:30]([F:32])([F:31])[F:33])=[CH:27][C:28](=[O:29])[N:23]([C:20]2[CH:21]=[CH:22][C:17]3[S:16][N:15]=[C:14]([C:13]([OH:47])=[O:12])[C:18]=3[CH:19]=2)[C:24]1=[O:35]

Komponenten

7

Edukt 3

HCID 24502Potassium DichromateHCID 178523685-[3,6-dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1, 2-benzisothiazole-3-carboxaldehydeHCID 221198213-[3-(hydroxymethyl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione

Produkt 1

HCID 11187860HCID 11187860, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittelHCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

A solution of potassium dichromate (10.0 g) in 1.5 M sulfuric acid (200 mL) is cooled to 0° C., treated dropwise with a solution of a 2:3 mixture of 3-[3-(hydroxymethyl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione and 5-[3,6-dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-carboxaldehyde (12.0 g) in acetic acid, stirred at room temperature for 2 hours, and diluted with water. The resultant aqueous mixture is extracted with methylene chloride. The organic extracts are combined, washed sequentially with water and brine, dried over anhydrous sodium sulfate, and concentrated in vacuo to give the title product as a white solid (8.50 g, mp 149-152° C.).

Aufarbeitung

  1. extractionThe resultant aqueous mixture is extracted with methylene chloride
  2. washwashed sequentially with water and brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-565e9ea917874e72a29ac18a98704b66
Quelldatensatz
uspto-grants-2004_03
Patentnummer
US06706663B2

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