反应详情

To a stirred solution of 3-(2-(dimethylamino)ethoxy)-1-methyl-1H-pyrazole-5-carboxylic acid (3.3 g, 15.5 mmol) and triethylamine (2.35 g, 23.2 mmol) in dry toluene (50 mL) was added DPPA (4.69 g, 17 mmol) under N2 and the mixture was refluxed for 1 hr. After the addition of benzyl alcohol (3.35 g, 31 mmol), the mixture was refluxed overnight. The mixture was concentrated in vacuo to give crude product, which was purified by column chromatography (silica gel, CH2Cl2/MeOH 30:1) to give the title compound (1.42 g, 29% yield) as a colorless oil.

1. temperaturethe mixture was refluxed for 1 hr
2. temperaturethe mixture was refluxed overnight
3. concentrationThe mixture was concentrated in vacuo
4. customto give crude product, which
5. customwas purified by column chromatography (silica gel, CH2Cl2/MeOH 30:1)