反应详情

温度

240 °C

To a stirred biphenyl-diphenyl ether eutectic (also called Dowtherm) (100 mL) at 240° C. under N2 was added 5-((1-(4-methoxybenzyl)-1H-pyrazol-5-ylamino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione (33.5 g, 93.7 mmol) in portions as a solid over a 10 minute period. After addition was complete, the mixture was heated at 240° C. for 10 minutes. After cooling to room temperature, the mixture was diluted with hexanes (300 mL), and the hexanes were decanted along with the majority of the Dowtherm. The remaining residue was diluted with diethyl ether (200 mL), and the ether was decanted from the residue and discarded. Lastly the residue was suspended in DCM (100 mL). The stirred suspension was diluted with diethyl ether (300 mL) and filtered. The resulting off-white solid (22.7 g, 91%) was dried under high vacuum. 1H NMR (400 MHz, DMSO-d6) δ 11.7 (br s, 1H), 8.17 (br s, 1H), 8.08 (s, 1H), 7.20 (d, J=9 Hz, 2H), 6.86 (d, J=9 Hz, 2H), 6.45 (br s, 1H), 5.50 (s, 2H), 3.70 (s, 3H).

1. additionAfter addition
2. temperatureAfter cooling to room temperature
3. customthe hexanes were decanted along with the majority of the Dowtherm
4. additionThe remaining residue was diluted with diethyl ether (200 mL)
5. customthe ether was decanted from the residue
6. additionThe stirred suspension was diluted with diethyl ether (300 mL)
7. filtrationfiltered
8. dry with materialThe resulting off-white solid (22.7 g, 91%) was dried under high vacuum