反应详情

温度

25 °C

To a suspension of NaH (14.7 g, 367 mmol) in DME (216 mL) was added dropwise a mixture of methyl 3-[2-(methyloxy)-5-pyrimidinyl]propanoate (18 g, 92 mmol) and methyl formate (33.1 g, 550 mmol) in DME (216 mL) under N2 at 0° C. The reaction mixture was stirred at 25° C. overnight, then filtered through a pad of Celite. The filtrate was diluted with ether (500 mL), kept standing for about 2 h and re-filtered. The filtrated cake was washed with diethyl ether and dried to give the title compound (14 g, 51.7%), which was used into next step without further purification.

1. additionwas added dropwise
2. filtrationfiltered through a pad of Celite
3. additionThe filtrate was diluted with ether (500 mL)
4. waitkept standing for about 2 h
5. filtrationre-filtered
6. washThe filtrated cake was washed with diethyl ether
7. customdried