Chlorosulfonic acid → HCID 87147127, compound

HRID 1026373Notes

Reaction equation

HRID 1026373 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]>C(OCC)(=O)C>[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

4

Reactant 2

HCID 24638Chlorosulfonic acidHCID 4581882,5-Dichlorobenzophenone

Product 1

HCID 87147127HCID 87147127, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

Into a 3 L three-neck flask equipped with a stirrer, and a cooling tube, chlorosulfonic acid (233.0 g, 2 mol) was added, and then 2,5-dichlorobenzophenone (100.4 g, 400 mmol) was added. The mixture was reacted for 8 hours using an oil bath at 100° C. After a predetermined period of time, the reaction liquid was slowly poured into broken ice (1000 g), and extraction using ethyl acetate was carried out. An organic layer was washed with a saline solution, and was dried with magnesium sulfate. Then, the ethyl acetate was distilled away, thereby obtaining a crude crystal of pale yellow (3-(2,5-dichlorobenzoyl)benzene sulfonic acid chloride). The crude crystal was employed at the subsequent step without purification.

Workup

  1. customInto a 3 L three-neck flask equipped with a stirrer, and a cooling tube
  2. customThe mixture was reacted for 8 hours
  3. customat 100° C
  4. waitAfter a predetermined period of time
  5. customthe reaction liquid
  6. washAn organic layer was washed with a saline solution
  7. dry with materialwas dried with magnesium sulfate
  8. distillationThen, the ethyl acetate was distilled away

Sources & evidence

ORD record
ord-650abd537f5747718f72c54f44310677
Source dataset
uspto-grants-2014_05
Patent number
US08729219B2

Reaction notes

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