Acetic Acid → 3-Carboxy-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyran

HRID 5358

Reaktionsgleichung

Reaktionsgleichung von HRID 5358
C([O:3][C:4]([C:6]1[C:11](=[O:12])[C:10]2[CH:13]=[C:14]([F:19])[C:15]([F:18])=[C:16]([F:17])[C:9]=2[S:8][C:7]=1[S:20][CH3:21])=[O:5])C.C(O)(=O)C.S(=O)(=O)(O)O>O>[C:4]([C:6]1[C:11](=[O:12])[C:10]2[CH:13]=[C:14]([F:19])[C:15]([F:18])=[C:16]([F:17])[C:9]=2[S:8][C:7]=1[S:20][CH3:21])([OH:5])=[O:3]

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 217702223-Ethoxycarbonyl-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyran

Produkt 1

HCID 197958433-Carboxy-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyranAusbeute 54 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 300 mg (0.897 mmol) of the compound of Example 111, 0.54 ml of acetic acid, 0.072 ml of concentrated sulfuric acid and 0.36 ml of water was stirred for 3 hours at 100° C. After cooling by allowing to stand, the crystals deposited were collected by filtration, washed with water, and dried to obtain 147 mg (0.481 mmol) of title compound (yield 54%).

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationthe crystals deposited were collected by filtration
  3. washwashed with water
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-1649d4530bee447eb356e4adaeb56455
Quelldatensatz
uspto-grants-1993_09
Patentnummer
US05244892

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