Реакция #4031

ord-fdcb81caf14240578e9ddd54ada0a201

Уравнение реакции

COC(=O)C(F)(F)C(F)(F)C(F)(F)F
Methyl perfluorobutyrate
C[Si](C)(C)[O-].[Na+]
sodium trimethylsilanolate
O=C([O-])C(F)(F)C(F)(F)C(F)(F)F.[Na+]
sodium perfluorobutyrate
Выход 84.0%

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияThe solid was filtered under nitrogen
  2. 2
    Промывкаwashed with dry ether
  3. 3
    Другоеdried under a stream of nitrogen

Методика

Methyl perfluorobutyrate (12.81 g, 56 mmol) was added dropwise to a stirred solution of sodium trimethylsilanolate (6.3 g, 56 mmol) in dry ether (300 mL) at room temperature under nitrogen. The reaction mixture was stirred overnight. The solid was filtered under nitrogen, washed with dry ether, and dried under a stream of nitrogen to afford sodium perfluorobutyrate (11.1 g, 84% yield) as a white solid: 19F NMR (D2O) δ -79.6 (t, J=8 Hz, CF3 --, 3F), -117.2 (q, J=8 Hz, CF3CF2CF2 --, 2F), -126.2 ppm (s, CF3CF2 --, 2F). Anal. Calcd. for C4F7NaO2 : C, 20.36; F, 56.35; Na, 9.74. Found: C, 20.84, 20.61, 20.58; F, 56.68, 53.24; Na, 9.89, 9.65.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04723016uspto-grants-1988_02