Methanol → Methyl-7-sulfamoyl-1,4-benzodioxane-5-carboxylate

HRID 1413137

Reaktionsgleichung

Reaktionsgleichung von HRID 1413137
S(=O)(=O)(O)O.[S:6]([C:10]1[CH:11]=[C:12]([C:20]([OH:22])=[O:21])[C:13]2[O:18][CH2:17][CH2:16][O:15][C:14]=2[CH:19]=1)(=[O:9])(=[O:8])[NH2:7].[CH3:23]O>>[CH3:23][O:21][C:20]([C:12]1[C:13]2[O:18][CH2:17][CH2:16][O:15][C:14]=2[CH:19]=[C:10]([S:6](=[O:8])(=[O:9])[NH2:7])[CH:11]=1)=[O:22]

Komponenten

4

Edukt 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 205447607-Sulfamoyl-2,3-dihydro-1,4-benzodioxine-5-carboxylic acid

Produkt 1

HCID 20544687Methyl-7-sulfamoyl-1,4-benzodioxane-5-carboxylateAusbeute 81,2 %

Versuchsvorschrift

429 g of methanol were introduced into a balloon flask provided with a condenser and then, under cooling, 54 g of 93% sulfuric acid and 111 g of 7-sulfamoyl-1,4-benzodioxane-5-carboxylic acid were added. The mixture was heated under reflux and then cooled. The crystals were dried off, washed with methanol and then treated with 500 cm3 of water and 5 g of sodium carbonate. The precipitate was dried off, washed with water and dried. 95 g of methyl-7-sulfamoyl-1,4-benzodioxane-5-carboxylate were obtained (M.P.: 225°-226° C.; yield: 81%).

Aufarbeitung

  1. customprovided with a condenser
  2. temperatureunder cooling
  3. temperatureThe mixture was heated
  4. temperatureunder reflux
  5. temperaturecooled
  6. customThe crystals were dried off
  7. washwashed with methanol
  8. additiontreated with 500 cm3 of water and 5 g of sodium carbonate
  9. customThe precipitate was dried off
  10. washwashed with water
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-89ce3f1c36f54410ae7c9b586a6b9cc0
Quelldatensatz
uspto-grants-1981_02
Patentnummer
US04248885

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