反应详情

5 g of 1-(3,4-dimethoxyphenyl)butane-1,3-dione (41) were initially introduced into 25 ml of acetic acid, and 1.71 g of sodium nitrite, dissolved in 5 ml of water, were then added dropwise at 15° C. The reaction solution was stirred at RT for 1 h and then remained standing for 2 h. 50 g of ice were added to the solution and the whole was then stored at 0° C. for 12 h, in connection with which the product precipitated out. The product was subsequently filtered off with suction and dried at 50° C. in a drying oven. The following was obtained: 42 C12H13NO5 (251.24); MS (ESI) 252 (M+H)

1. additionwere then added dropwise at 15° C
2. waitremained standing for 2 h
3. waitthe whole was then stored at 0° C. for 12 h, in connection with which
4. customthe product precipitated out
5. filtrationThe product was subsequently filtered off with suction
6. customdried at 50° C. in a drying oven
7. customThe following was obtained