Реакция #56216

ord-e5fa55e5d11d47038609d1a40afb8733

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураis refluxed for 11/2 hours
  2. 2
    Другоеthe water and excess hydrazine are removed by a takeoff condenser until the temperature
  3. 3
    Другоеrises to 195°-200°
  4. 4
    Температураthe solution is cooled
  5. 5
    workup.ADDITIONpoured into ice and water (50 ml)
  6. 6
    Экстракцияextracted with ether (3×20 ml)
  7. 7
    ПромывкаThe combined ether layers are washed with water (3×20 ml), brine (10 ml)
  8. 8
    Сушкаdried over calcium sulfate
  9. 9
    ДругоеRemoval of solvents

Методика

A mixture of (6-benzoyl-2-pyridyl)methanol (1.5 g, 7 mmol), potassium hydroxide (1.3 g, 23 mmol) and hydrazine 85% (1 ml, 25 mmol) in triethylene glycol (10 ml) is refluxed for 11/2 hours, and then the water and excess hydrazine are removed by a takeoff condenser until the temperature rises to 195°-200°. After 4 hours at 195°-200°, the solution is cooled, poured into ice and water (50 ml) and extracted with ether (3×20 ml). The combined ether layers are washed with water (3×20 ml), brine (10 ml) and dried over calcium sulfate. Removal of solvents gives (6-benzyl-2-pyridyl)methanol.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04224330uspto-grants-1980_09