반응 #1435732

ord-23fce526404044e9a47c6e0dc7f178da

반응 방정식

Cc1nc2nccn2c(O)c1-c1c(F)cccc1Cl
5-hydroxy-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine
CCN(CC)c1ccccc1
N,N-diethylaniline
O=P(Cl)(Cl)Cl
phosphorus oxychloride
Cc1nc2nccn2c(Cl)c1-c1c(F)cccc1Cl
5-chloro-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed
  2. 2
    온도under heating for 26 hours
  3. 3
    농축The reaction mixture was concentrated
  4. 4
    workup.ADDITIONdichloromethane and aqueous saturated sodium bicarbonate solution were added to the residue
  5. 5
    세척The separated organic layer was washed with water
  6. 6
    건조dried over sodium sulfate
  7. 7
    농축concentrated

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07211545B2uspto-grants-2007_05