반응 #1492060

ord-6352577f1c45465290f2269cd7033acd

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타an organic layer was separated from the resultant solution
  2. 2
    추출an aqueous layer was subjected to extraction with 6.5 parts of chloroform
  3. 3
    세척washed with an ion-exchanged water
  4. 4
    농축the obtained organic layer was concentrated
  5. 5
    workup.ADDITIONTo the concentrated solution, 5.0 parts of tert-butyl methyl ether was added
  6. 6
    workup.STIRRINGthe resultant mixture was stirred
  7. 7
    여과filtered

실험 절차

To a obtained solution of the sodium salt of 3-hydroxy-1-adamantylmethyl difluorosulfoacetate, 17.2 parts of chloroform, and 2.9 parts of a 14.8 mass % aqueous triphenyl sulfonium chloride solution were added, and the mixture was stirred for 15 hours, and then an organic layer was separated from the resultant solution, and an aqueous layer was subjected to extraction with 6.5 parts of chloroform. Organic layers were combined and washed with an ion-exchanged water, and the obtained organic layer was concentrated. To the concentrated solution, 5.0 parts of tert-butyl methyl ether was added, and the resultant mixture was stirred and filtered to obtain, as a white solid, 0.2 parts of triphenylsulfonium 1-((3-hydroxy-1-adamantyl)methoxycarbonyl)difluoromethane sulfonate (B1-2).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08916330B2uspto-grants-2014_12