Реакция #1435732

ord-23fce526404044e9a47c6e0dc7f178da

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwas refluxed
  2. 2
    Температураunder heating for 26 hours
  3. 3
    КонцентрированиеThe reaction mixture was concentrated
  4. 4
    workup.ADDITIONdichloromethane and aqueous saturated sodium bicarbonate solution were added to the residue
  5. 5
    ПромывкаThe separated organic layer was washed with water
  6. 6
    Сушкаdried over sodium sulfate
  7. 7
    Концентрированиеconcentrated

Методика

A mixture of 0.16 g of 5-hydroxy-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine, 0.20 g of N,N-diethylaniline and 2 ml of phosphorus oxychloride was refluxed under heating for 26 hours. The reaction mixture was concentrated, and dichloromethane and aqueous saturated sodium bicarbonate solution were added to the residue. The separated organic layer was washed with water, dried over sodium sulfate and concentrated. The residue was subjected to silica gel chromatography to give 45mg of 5-chloro-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07211545B2uspto-grants-2007_05