تفاعل #2200

ord-9900c0905406446f8afdb6d500c86aee

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةgradually heated
  2. 2
    workup.STIRRINGThe mixture was stirred for 4 hours
  3. 3
    درجة الحرارةunder reflux
  4. 4
    workup.WAITleft
  5. 5
    درجة الحرارةto cool
  6. 6
    workup.DISTILLATIONThen, the solvent was distilled off under reduced pressure
  7. 7
    أخرىThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1)

الإجراء التجريبي

4-chloro-4'-ethane sulfonylmethylbenzhydrol (6.0 g), thionyl chloride (5.4 g), toluene (200 ml) and a catalytic amount of N,N-dimethylformamide were mixed and gradually heated with stirring to a refluxing temperature. The mixture was stirred for 4 hours under reflux and then left to cool. Then, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1) to obtain the desired product as a slight yellow viscous substance (4.6 g, nD20 : 1.6044, yield: 75%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05728699uspto-grants-1998_03