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Acetic Anhydride → N-(2-chloro-4-fluorophenyl)-N-[(chloromethyl)sulfonyl]acetamide

HRID 432961
Notes
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Reaction equation

HRID 432961 reaction equation
[Cl:1][CH2:2][S:3]([NH:6][C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][C:8]=1[Cl:14])(=[O:5])=[O:4].[C:15](OC(=O)C)(=[O:17])[CH3:16]>>[Cl:14][C:8]1[CH:9]=[C:10]([F:13])[CH:11]=[CH:12][C:7]=1[N:6]([S:3]([CH2:2][Cl:1])(=[O:4])=[O:5])[C:15](=[O:17])[CH3:16]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 2

HCID 7918Acetic AnhydrideHCID 187608471-chloro-N-(2-chloro-4-fluorophenyl)methanesulfonamide

Product 1

HCID 18760837N-(2-chloro-4-fluorophenyl)-N-[(chloromethyl)sulfonyl]acetamideYield 80%

Procedure

77.5 g (0.3 mol) of 1-chloro-N-(2-chloro-4-fluorophenyl)methanesulfonamide were dissolved in 204.2 g (2 mol) of acetic anhydride and refluxed for 4 hours. The excess acetic anhydride was distilled off under reduced pressure at 100° C. To the still hot residue was added ethanol with stirring and the product precipitated (seeding may aid in crystallization). The crude product was filtered off and washed with cold ethanol and dried to yield 72 g (80%) of the title compound as a solid melting at 89-92° C.

Workup

  1. temperaturerefluxed for 4 hours
  • distillationThe excess acetic anhydride was distilled off under reduced pressure at 100° C
  • additionTo the still hot residue was added ethanol
  • customthe product precipitated
  • custom(seeding may aid in crystallization)
  • filtrationThe crude product was filtered off
  • washwashed with cold ethanol
  • customdried
  • Sources & evidence

    ORD record
    ord-736b0b335daa45758f4be717cbaf4c5c
    Source dataset
    uspto-grants-2003_12
    DOI
    10.6084/m9.figshare.5104873.v1
    Patent number
    US06664400B2

    Reaction notes

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    On this pageParticipantsProcedureWorkupSources & evidenceReaction notes