Ethyl sulfate anion → HCID 20544726, compound

HRID 127398Notes

Reaction equation

HRID 127398 reaction equation
[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]

Participants

4

Reactant 2

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

Product 1

HCID 20544726HCID 20544726, compoundYield 81%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

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 100 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%).

Workup

  1. customprovided with a condenser
  2. temperatureThe mixture was heated
  3. temperatureunder reflux
  4. temperaturecooled
  5. filtrationfiltered
  6. additiontreated with 100 cm3 of hydrochloric acid
  7. customThe precipitate was dried off
  8. washwashed with water
  9. customdried

Sources & evidence

ORD record
ord-ee2d55753a374e7387e2c31e6f93703c
Source dataset
uspto-grants-1981_03
Patent number
US04255580

Reaction notes

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