تفاعل #59819

ord-ba8804115d7f438d8e16948d3df34747

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGThe mixture was stirred at room temperature for 2 hours
  2. 2
    استخلاصthe aqueous layer was extracted twice with dichloromethane
  3. 3
    أخرىdried
  4. 4
    ترشيحfiltered
  5. 5
    تركيزThe filtrate was concentrated
  6. 6
    أخرىthe residue was purified by silica gel column chromatography

الإجراء التجريبي

Under nitrogen atmosphere, to a suspension of aluminum chloride (4.62 g, 34.7 mmol) in ethylene chloride (50 mL) was added a solution of p-toluoyl chloride (4.91 g, 31.8 mmol) in ethylene chloride (5 mL) at room temperature over a period of 10 minutes. The mixture was stirred for 30 minutes, and thereto was added a solution of 1-benzenesulfonyl-1H-pyrrole (6.00 g, 28.9 mmol) in ethylene chloride (10 mL) over a period of 10 minutes. The mixture was stirred at room temperature for 2 hours. The reaction mixture was poured into ice-water, and the aqueous layer was extracted twice with dichloromethane. The organic layers were combined, dried, and filtered. The filtrate was concentrated, and the residue was purified by silica gel column chromatography to give the title compound (9.9 g, 100%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07425642B2uspto-grants-2008_09