反应详情

A mixture of 1.6g of 2-isopropylpyrazolo[1,5-a]pyridine and 2.1g of N,N-dimethylcarbamoyl chloride was dissolved in 20 ml of nitrobenzene. Four grams of aluminum chloride (powder) was added at room-temperature to the resulting solution and reaction mixture was refluxed for 8 hr and concentrated under reduced pressure. Water was added to the residue and the mixture was made basic with potassium hydroxide solution, extracted with chloroform. The chloroform solution was dried over sodium sulfate and concentrated. The residue was column chromatographed over aluminum to give objective product. Distillation gave colorless oil, bp 175° (2 mmHg). Yield 1.1g (50%).

1. temperaturewas refluxed for 8 hr
2. concentrationconcentrated under reduced pressure
3. additionWater was added to the residue
4. extractionextracted with chloroform
5. dry with materialThe chloroform solution was dried over sodium sulfate
6. concentrationconcentrated
7. customchromatographed over aluminum
8. customto give objective product
9. distillationDistillation
10. customgave colorless oil, bp 175° (2 mmHg)