تفاعل #1354128

ord-fa2c7b0be44b4d69909bbd8d7c65606c

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe organic layer was separated
  2. 2
    غسيلwashed with 400 g of water
  3. 3
    تركيزconcentrated in vacuum
  4. 4
    أخرىThe residue, 150 g, was purified by silica gel column chromatography (eluent, dichloromethane/methanol)

الإجراء التجريبي

The sodium 3-methoxy-4-(4′-methylphenylsulfonyloxy)-benzenesulfonate crude product obtained in Synthesis Example 1, 90 g, was added to the aqueous triphenylsulfonium chloride solution obtained in Synthesis Example 2 and 400 g of dichloromethane, which was stirred for one hour at room temperature. The organic layer was separated, washed with 400 g of water, and concentrated in vacuum. The residue, 150 g, was purified by silica gel column chromatography (eluent, dichloromethane/methanol), obtaining the end product, triphenylsulfonium 3-methoxy-4-(4′-methylphenyl-sulfonyloxy)benzenesulfonate as an oily matter in an amount of 69 g (yield 56%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06551758B2uspto-grants-2003_04