تفاعل #3043

ord-5ea8ac69bd1848ae813a64e74a7a7adf

المذيبات

ظروف التفاعل

درجة الحرارة
-4°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe mixture separated into layers which
  2. 2
    أخرىwere subsequently separated
  3. 3
    غسيلThe organic layer was washed with 100 ml of saturated sodium bicarbonate and 100 ml of brine
  4. 4
    أخرىThe organic layer was dried
  5. 5
    أخرىthe solvent evaporated

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05731336uspto-grants-1998_03