반응 #1354128

ord-fa2c7b0be44b4d69909bbd8d7c65606c

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06551758B2uspto-grants-2003_04