반응 #2146695

ord-5610be1c99b34922ad05dbfcc85590fa

반응 방정식

O=C(CBr)c1ccc(O)cc1
2-bromo-4′-hydroxyacetophenone
Nc1ccccn1
2-aminopyridine
O=C([O-])O.[Na+]
sodium hydrogencarbonate
Oc1ccc(-c2cn3ccccc3n2)cc1
2-(4′-hydroxyphenyl)imidazo[1,2-a]pyridine
수율 63.3%

반응 조건

온도
110°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After the reaction solution was cooled down to room temperature
  2. 2
    온도The resulting mixture was refluxed in an oil bath at 100° C. for one hour
  3. 3
    기타After the completion of the reaction
  4. 4
    온도the reaction solution was cooled to room temperature
  5. 5
    기타precipitates
  6. 6
    여과were filtered
  7. 7
    기타recovered
  8. 8
    세척The precipitates were washed with acetonitrile and water
  9. 9
    기타dried under reduced pressure

실험 절차

649 mg (corresponding to 3.0 mmol) of 2-bromo-4′-hydroxyacetophenone and 285 mg (corresponding to 3.0 mmol) of 2-aminopyridine were dissolved in 20 mL of acetonitrile. The resulting solution was refluxed in an oil bath at 110° C. for one hour. After the reaction solution was cooled down to room temperature, 254 mg (corresponding to 5.4 mmol) of sodium hydrogencarbonate was added thereto. The resulting mixture was refluxed in an oil bath at 100° C. for one hour. After the completion of the reaction, the reaction solution was cooled to room temperature, and precipitates were filtered and recovered therefrom. The precipitates were washed with acetonitrile and water, and then dried under reduced pressure to obtain 405 mg (corresponding to 1.9 mmol) of 2-(4′-hydroxyphenyl)imidazo[1,2-a]pyridine (FIG. 4, Step 2).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08277777B2uspto-grants-2012_10