Chlorosulfonic acid → HCID 87147127, compound

HRID 2389227Notes

Reaction equation

HRID 2389227 reaction equation
[Cl:1][S:2]([OH:5])(=O)=[O:3].[Cl:6][C:7]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:8]=1[C:9]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[O:10]>>[Cl:6][C:7]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:8]=1[C:9]([C:11]1[CH:16]=[C:15]([S:2]([Cl:1])(=[O:5])=[O:3])[CH:14]=[CH:13][CH:12]=1)=[O:10]

Participants

3

Procedure

Chlorosulfonic acid (233.0 g, 2 mol) was added into a 3 L three-necked flask equipped with a stirrer and cooling pipe, followed by adding 2,5-dichlorobenzophenone (100.4 g, 400 mmol), and the reactant was allowed to react for 8 hours using an oil bath at 100° C. After a predetermined time, the reaction liquid was slowly poured into crushed ice (1000 g) and extracted with ethyl acetate. The organic layer was washed with sodium chloride solution and dried with magnesium sulfate, and then ethyl acetate was removed to obtain a light yellow crude crystal (3-(2,5-dichlorobenzoyl)benzenesulfonic acid chloride. The crude crystal was not purified and directly used in the following step.

Workup

  1. customequipped with a stirrer
  2. temperaturecooling pipe
  3. customto react for 8 hours
  4. customat 100° C
  5. customAfter a predetermined time, the reaction liquid
  6. additionwas slowly poured
  7. extractionextracted with ethyl acetate
  8. washThe organic layer was washed with sodium chloride solution
  9. dry with materialdried with magnesium sulfate
  10. customethyl acetate was removed

Sources & evidence

ORD record
ord-826b27c7e1274c3bb1ce13ff174e21a6
Source dataset
uspto-grants-2012_09
Patent number
US08273499B2

Reaction notes

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