Chlorosulfonic acid → HCID 20062876, compound

HRID 1084923Notes

Reaction equation

HRID 1084923 reaction equation
[O:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][C:9]=2[C:11]([OH:13])=[O:12])[CH2:4][CH2:3][CH2:2]1.[Cl:14][S:15](O)(=[O:17])=[O:16]>>[Cl:14][S:15]([C:7]1[CH:6]=[C:5]2[C:10](=[C:9]([C:11]([OH:13])=[O:12])[CH:8]=1)[O:1][CH2:2][CH2:3][CH2:4]2)(=[O:17])=[O:16]

Participants

3

Reactant 2

HCID 24638Chlorosulfonic acidHCID 127011383,4-Dihydro-2H-1-benzopyran-8-carboxylic acid

Product 1

HCID 20062876HCID 20062876, compound

Conditions

Temperature
10 °C

Procedure

930 ml of chlorosulphonic acid were introduced into a 1-liter round-bottomed flask and 165 g of chroman-8-carboxylic acid were then added in small amounts, while maintaining the temperature between 0° C. and 10° C. by cooling. The solution was stirred for 1 hour at 10° C., and then allowed to stand overnight at ambient temperature. It was then poured in small amounts onto ice, while stirring and maintaining the temperature at 0° C. by cooling externally and by introducing ice into the flask.

Workup

  1. temperaturewhile maintaining the temperature between 0° C. and 10° C.
  2. temperatureby cooling
  3. waitto stand overnight at ambient temperature
  4. additionIt was then poured in small amounts onto ice
  5. stirringwhile stirring
  6. temperaturemaintaining the temperature at 0° C.
  7. temperatureby cooling externally
  8. additionby introducing ice into the flask

Sources & evidence

ORD record
ord-5fa4fc8f909f4345a9e17994857f68f8
Source dataset
uspto-grants-1991_04
Patent number
US05006570

Reaction notes

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