Реакция #2380643

ord-9a661326f33d4d0abaead365952d41dd

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураto cool
  2. 2
    Фильтрацияthe solid is filtered off
  3. 3
    Промывкаwashed with water
  4. 4
    Другоеdried
  5. 5
    Другоеevaporated down
  6. 6
    Фильтрацияthe precipitated pale brown solid is filtered off

Методика

Under a nitrogen blanket and at 90° C., 2 g (9.2 mmol) of the acetylene derivative from Example 1 is added to a mixture of 50 mg of copper(II) chloride, 110 mg of palladium(II) acetate, 380 mg of triphenylphosphine and 2.6 g (18.4 mmol) of benzoyl chloride in 100 ml of triethylamine. After 30 minutes, the mixture is allowed to cool and the solid is filtered off. The filtrate is evaporaed down, and the residue is taken up in methyl tert-butyl ether, washed with water, dried and evaporated down. The residue is stirred with diethyl ether and the precipitated pale brown solid is filtered off. 2.0 g (68%) of compound 26, Table 6, remain. Mp. 89°-94° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05686474uspto-grants-1997_11