تفاعل #1435732

ord-23fce526404044e9a47c6e0dc7f178da

معادلة التفاعل

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

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed
  2. 2
    درجة الحرارةunder heating for 26 hours
  3. 3
    تركيزThe reaction mixture was concentrated
  4. 4
    workup.ADDITIONdichloromethane and aqueous saturated sodium bicarbonate solution were added to the residue
  5. 5
    غسيلThe separated organic layer was washed with water
  6. 6
    تجفيفdried over sodium sulfate
  7. 7
    تركيزconcentrated

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07211545B2uspto-grants-2007_05