Реакция #10880

ord-ff4256aaf0c04c6c9ceb8c97dc41cecd

Уравнение реакции

CCOP([O-])OCC
diethylphosphite
CCN(CC)CC
triethylamine
O=C(c1ccc(N2CCCCC2)cc1)C(Br)Br
2,2-Dibromo-1-[4-(1-piperidinyl)phenyl]ethanone
O=C(c1ccc(N2CCCCC2)cc1)C(Br)Br
2,2-dibromo-1-[4-(1-piperidinyl)phenyl]ethanone
O=C(CBr)c1ccc(N2CCCCC2)cc1
2-bromo-1-[4-(1-piperidinyl)phenyl]ethanone
Выход 100.0%

Растворители

Условия реакции

Температура
0°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe mixture was slowly warmed to room temperature
  2. 2
    workup.STIRRINGstirred for 6 h
  3. 3
    КонцентрированиеThe reaction mixture was concentrated in vacuo
  4. 4
    workup.ADDITIONpoured into ice/water
  5. 5
    ФильтрацияThe precipitate was collected by filtration
  6. 6
    Промывкаwashed with water
  7. 7
    Другоеdried in vacuo

Методика

2,2-Dibromo-1-[4-(1-piperidinyl)phenyl]ethanone (3 g, 8.3 mmol) (from Step A above) was dissolved in tetrahydrofuran (15 mL), and cooled to 0° C. To the resulting solution were added dropwise diethylphosphite (1.13 mL, 8.7 mmol) and triethylamine (1.21 mL, 8.7 mmol) in tetrahydrofuran (7 mL) at 0° C. with stirring. The mixture was slowly warmed to room temperature and stirred for 6 h. The reaction mixture was concentrated in vacuo and poured into ice/water. The precipitate was collected by filtration, washed with water and dried in vacuo to provide 2-bromo-1-[4-(1-piperidinyl)phenyl]ethanone (2.3 g, 100% yield).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07094896B2uspto-grants-2006_08