반응 #3043

ord-5ea8ac69bd1848ae813a64e74a7a7adf

반응 조건

온도
-4°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The mixture separated into layers which
  2. 2
    기타were subsequently separated
  3. 3
    세척The organic layer was washed with 100 ml of saturated sodium bicarbonate and 100 ml of brine
  4. 4
    기타The organic layer was dried
  5. 5
    기타the solvent evaporated

실험 절차

Under a nitrogen atmosphere, 6.89 ml of acetylchloride and 14.75 ml of stannic chloride were dissolved in 200 ml of methylene chloride and chilled to -4° C. To this was added 20 g of 2,6-di-t-butylphenol (in 100 ml of methylene chloride) over 10 minutes. The resultant mixture was stirred for 30 minutes at 0° C., then poured into a mixture of 400 ml of ice and 1N hydrochloric acid and stirred. The mixture separated into layers which were subsequently separated. The organic layer was washed with 100 ml of saturated sodium bicarbonate and 100 ml of brine. The organic layer was dried and the solvent evaporated to give 23.39 g of the desired subtitled intermediate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05731336uspto-grants-1998_03