Réaction #684132

ord-05fcd04d5e784832879799e157b6d233

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurecooling with ice
  2. 2
    workup.STIRRINGwhole stirred for 2 hours at room temperature
  3. 3
    FiltrationThe solution is filtered
  4. 4
    Concentrationthe filtrate concentrated at 0.01 mm and a bath temperature of 40° C
  5. 5
    Lavagewashed with cold aqueous NaNHCO3 solution
  6. 6
    SéchageThe organic phase is dried over Na2SO4
  7. 7
    workup.DISTILLATIONdistilled 20 parts of chloromethylbenzoyl sulfide having a boiling point at 0.1 mm of 111° to 113° C
  8. 8
    Autreis obtained

Mode opératoire

42 PARTS OF PHOSPHORUS PENTACHLORIDE IS COVERED WITH A LAYER OF ABSOLUTE ETHER. While stirring and cooling with ice, an ethereal solution of 33.6 parts of hydroxymethylbenzoyl sulfide is dripped in and the whole stirred for 2 hours at room temperature. The solution is filtered, the filtrate concentrated at 0.01 mm and a bath temperature of 40° C, the residue taken up in methylene chloride and washed with cold aqueous NaNHCO3 solution. The organic phase is dried over Na2SO4 and distilled 20 parts of chloromethylbenzoyl sulfide having a boiling point at 0.1 mm of 111° to 113° C is obtained.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US04012521uspto-grants-1977_03