Methanol → Methyl-8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxylate

HRID 1660019Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1660019
CO.S(=O)(=O)(O)O.[CH3:8][O:9][C:10]1[C:15]2[O:16][CH2:17][CH2:18][O:19][C:14]=2[C:13]([C:20]([OH:22])=[O:21])=[CH:12][C:11]=1[S:23](=[O:26])(=[O:25])[NH2:24].[C:27](=O)([O-])[O-].[Na+].[Na+]>O>[CH3:27][O:21][C:20]([C:13]1[C:14]2[O:19][CH2:18][CH2:17][O:16][C:15]=2[C:10]([O:9][CH3:8])=[C:11]([S:23](=[O:26])(=[O:25])[NH2:24])[CH:12]=1)=[O:22]

Komponenten

6

Edukt 4

HCID 887MethanolHCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 205446908-Methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxylic acid

Produkt 1

HCID 20544706Methyl-8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxylateAusbeute 96,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

396 g of methanol were introduced into a balloon flask provided with a condenser and then 51 g of sulfuric acid and 114.5 g of 8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxylic acid were added while cooling. The mixture was heated under reflux and then poured into 485 cm3 of water and 40 g of sodium carbonate. The precipitate was dried off, washed and dried. 110.5 g of methyl-8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxylate were obtained (M.P.: 202°-203° C.; yield: 92%).

Aufarbeitung

  1. customprovided with a condenser
  2. temperaturewhile cooling
  3. temperatureThe mixture was heated
  4. temperatureunder reflux
  5. customThe precipitate was dried off
  6. washwashed
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-fd4c7f3483dd4a05ad19f89e37d4e1bf
Quelldatensatz
uspto-grants-1981_12
Patentnummer
US04306072

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