反应详情

To a suspension of sodium hydrate (0.228 g, 60%, 5.72 mmole) in 15 ml DMF was added nitrile (IV) (1.2 g, 3.9 mmole ) and after stirring for 15 minutes at room temperature 1,2-dibromo-ethane (1.1 g, 5.8 mmole ) in 1.5 ml DMF was added. The resulting mixture was stirred 0.5 hour at room temperature and then more sodium hydrate (0.114 g, 2.86 mmole ) was added and the reaction mixture heated for about 10 minutes at 30-35° C. After cooling the mixture was partitioned between ethylacetate and brine, the organic layer was dried over sodium acetate and concentrated in vacuo. Purification by silica gel column chromatography with 30% -50% ethylacetate in hexane afforded compound (V ) 1 g (77% yield).

1. additionwas added
2. temperaturethe reaction mixture heated for about 10 minutes at 30-35° C
3. temperatureAfter cooling the mixture
4. customwas partitioned between ethylacetate and brine
5. dry with materialthe organic layer was dried over sodium acetate
6. concentrationconcentrated in vacuo