Ethyl sulfate anion → 7-Ethylthio-1,4-benzodioxane-5-carboxylic acid

HRID 2052616Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2052616
[SH:1][C:2]1[CH:3]=[C:4]([C:12]([OH:14])=[O:13])[C:5]2[O:10][CH2:9][CH2:8][O:7][C:6]=2[CH:11]=1.[CH2:15](OS([O-])(=O)=O)[CH3:16]>O>[CH2:15]([S:1][C:2]1[CH:3]=[C:4]([C:12]([OH:14])=[O:13])[C:5]2[O:10][CH2:9][CH2:8][O:7][C:6]=2[CH:11]=1)[CH3:16]

Komponenten

4

Edukt 2

HCID 3804841Ethyl sulfate anionHCID 205446947-Mercapto-1,4-benzodioxane-5-carboxylic acid

Produkt 1

HCID 205447267-Ethylthio-1,4-benzodioxane-5-carboxylic acidAusbeute 81 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

166 g of 7-mercapto-1,4-benzodioxane-5-carboxylic acid, 242 cm3 of water, 216 cm3 of soda lye and 181 g of ethylsulfate were introduced into a balloon flask provided with a condenser. The mixture was heated under reflux and then cooled. The solution was poured into 1.3 l of water, filtered and treated with 110 cm3 of hydrochloric acid. The precipitate was dried off, washed with water and dried. 152 g of 7-ethylthio-1,4-benzodioxane-5-carboxylic acid were obtained (M.P.: 153°-154° C.; yield: 81%).

Aufarbeitung

  1. customprovided with a condenser
  2. temperatureThe mixture was heated
  3. temperatureunder reflux
  4. temperaturecooled
  5. filtrationfiltered
  6. additiontreated with 110 cm3 of hydrochloric acid
  7. customThe precipitate was dried off
  8. washwashed with water
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-c1fffb67295d4e88aae5c695c338df30
Quelldatensatz
uspto-grants-1980_01
Patentnummer
US04186135

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