Hydrochloric Acid → HCID 11480951, compound

HRID 431277Notes

Reaction equation

HRID 431277 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.Cl[S:10]([OH:13])(=[O:12])=[O:11].Cl>C(Cl)(Cl)Cl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([S:10]([OH:13])(=[O:12])=[O:11])[CH:3]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 97324-FluorophenolHCID 24638Chlorosulfonic acid

Product 1

HCID 11480951HCID 11480951, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

200 g (1.78 mol) of 4-fluorophenol are dissolved under a nitrogen atmosphere in 1300 ml of CHCl3 (distilled, dried over CaCl2). Added dropwise to this solution, over a period of 1 hour at room temperature with stirring, are 131 ml(229 g=1.96 mol) of chlorosulfonic acid, a vigorous release of HCl being observed initially, which dies down 30 min after completion and ceases entirely after a further 3 hours. After a reaction time of 24 hours, the precipitated product is filtered off with suction at room temperature under inert gas, washed twice with 200 ml of CHCl3 each time, and dried in vacuo at 1333 Pa and room temperature for 3 hours.

Workup

  1. additionAdded dropwise to this solution, over a period of 1 hour at room temperature
  2. waitafter completion and ceases entirely after a further 3 hours
  3. filtrationAfter a reaction time of 24 hours, the precipitated product is filtered off with suction at room temperature under inert gas
  4. washwashed twice with 200 ml of CHCl3 each time
  5. customdried in vacuo at 1333 Pa and room temperature for 3 hours

Sources & evidence

ORD record
ord-26a85b363a184c888ba0822e3008c4c1
Source dataset
uspto-grants-2003_12
Patent number
US06657072B2

Reaction notes

Loading…