تفاعل #2146695

ord-5610be1c99b34922ad05dbfcc85590fa

معادلة التفاعل

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
المردود 63.3%

المذيبات

ظروف التفاعل

درجة الحرارة
110°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter the reaction solution was cooled down to room temperature
  2. 2
    درجة الحرارةThe resulting mixture was refluxed in an oil bath at 100° C. for one hour
  3. 3
    أخرىAfter the completion of the reaction
  4. 4
    درجة الحرارةthe reaction solution was cooled to room temperature
  5. 5
    أخرىprecipitates
  6. 6
    ترشيحwere filtered
  7. 7
    أخرىrecovered
  8. 8
    غسيلThe precipitates were washed with acetonitrile and water
  9. 9
    أخرىdried under reduced pressure

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08277777B2uspto-grants-2012_10