Реакция #73809

ord-1401f71a1cf34abdb7b46f1046ccce95

Растворители

Условия реакции

Температура
-15°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураbefore warming to room temperature over 1 hour
  2. 2
    ДругоеThe reaction mixture was quenched with water
  3. 3
    Экстракцияextracted with diethyl ether, organic extracts
  4. 4
    Сушкаdried (MgSO4)
  5. 5
    Концентрированиеconcentrated

Методика

n-Butyllithium (0.47 ml, 0.76 mmol, 1.6M in Hexanes) was added dropwise to a solution of (R)(Diphenyl-phosphinoylmethyl)-methyl-(1-phenyl-ethyl)-amine* (0.18 g, 0.51 mmol) in dry tetrahydrofuran (9 ml) at −15° C. After 15 minutes a solution of (4-Chloro-phenyl)-[6-(3-methyl-1-trityl-1H-pyrazol-4-yl)-pyridin-3-yl]-methanone (0.14 g, 0.25 mmol) in tetrahydrofuran (0.9 ml) was added and the reaction mixture was stirred for a further 30 minutes at −15° C. before warming to room temperature over 1 hour. The reaction mixture was quenched with water, extracted with diethyl ether, organic extracts were combined, dried (MgSO4) and concentrated to afford the title compound, which was used in the next step without further purification.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08541461B2uspto-grants-2013_09