تفاعل #83218
ord-1eb6773bd68e43db9cb10fb39ab16f0c
معادلة التفاعل
الكواشف
ظروف التفاعل
المعالجة
- 1workup.STIRRINGAfter stirring of the mixture for 1 hour at ambient temperature
- 2استخلاصthe separated oil was extracted with dichloromethane
- 3غسيلThe extract was washed with brine
- 4أخرىdried
- 5تركيزconcentrated in vacuo
- 6workup.DISSOLUTIONThe residue was dissolved in a solution of sodium (138 mg) in ethanol (5 ml)
- 7درجة الحرارةthe solution was refluxed for 1 hour
- 8درجة الحرارةThe reaction mixture was cooled
- 9workup.ADDITIONpoured into water and neutralized with diluted hydrochloric acid
- 10استخلاصThe separated oil was extracted with dichloromethane
- 11غسيلthe extract was washed with brine
- 12أخرىdried
- 13تركيزconcentrated in vacuo
- 14أخرىThe residue was crystallized from ethanol
الإجراء التجريبي
To a suspension of sodium hydride (288 mg) in N,N-dimethylformamide (20 ml) was added dropwise a solution of 5-amino-3-(4-fluorophenyl)-4-(pyridin-4-yl)pyrazole (1.524 g) in N,N-dimethylformamide (5 ml) with ice cooling. The mixture was stirred for 30 minutes and to the mixture was added a solution of ethyl chloroacetate (883 mg) in N,N-dimethylformamide (5 ml). After stirring of the mixture for 1 hour at ambient temperature, the reaction mixture was poured into water and the separated oil was extracted with dichloromethane. The extract was washed with brine, dried and concentrated in vacuo. The residue was dissolved in a solution of sodium (138 mg) in ethanol (5 ml) and the solution was refluxed for 1 hour. The reaction mixture was cooled, poured into water and neutralized with diluted hydrochloric acid. The separated oil was extracted with dichloromethane and the extract was washed with brine, dried and concentrated in vacuo. The residue was crystallized from ethanol to yield 2,3-dihydro-6-(4-fluorophenyl)-2-oxo-7-(pyridin-4-yl)-1H-imidazo[1,2-b]pyrazole (178 mg).