反应详情

To a suspension of NaH (5.2 g, 130 mmol) in DMF/THF (110 ml/45 ml) was added diethyl malonate (19 ml, 125 mmol) dropwise and the mixture was stirred for 30 min at room temperature. To the mixture was added 2-(Bromomethyl)-1-fluoro-3-nitrobenzene (29 g, 124 mmol) in DMF/THF (40 ml/30 ml) and the resulting mixture was refluxed for 3 h. After cooling, the excess reagent was quenched with brine and the mixture was extracted with ethyl acetate. The extract was dried over sodium sulfate and concentrated in vacuo to afford diethyl 2-(2-Fluoro-6-nitrobenzyl)malonate (48 g) as a brown oil. This crude product was used in the next step without further purification.

1. temperaturethe resulting mixture was refluxed for 3 h
2. temperatureAfter cooling
3. customthe excess reagent was quenched with brine
4. extractionthe mixture was extracted with ethyl acetate
5. dry with materialThe extract was dried over sodium sulfate
6. concentrationconcentrated in vacuo