反应详情

温度

0 °C

To a solution of Compound 1 (2.0 g, 3.19 mmol) obtained in Example 1 in 30 ml of N,N-dimethylformamide was portionwise added sodium hydride (60% in oil, 270 mg, 6.71 mmol) with stirring at 0° C., and 2-dimethylaminoethylchloride hydrochloride (460 mg, 3.19 mmol) was added thereto, followed by heating to 80° C. and then stirring for one hour. A saturated aqueous solution of ammonium chloride was added to the reaction solution for neutralization, and water was added thereto followed by extraction with ethyl acetate. The resulting organic layer was washed with a saturated aqueous solution of sodium chloride and dried over magnesium sulfate, and the solvent was distilled off under reduced pressure to give 2.9 g of a crude product. The obtained crude product was purified with silica gel column chromatography (ethyl acetate/hexane=1/1-ethyl acetate alone) to give 2.1 g (yield: 94%) of the title compound.

1. temperatureby heating to 80° C.
2. stirringstirring for one hour
3. additionwas added
4. extractionthereto followed by extraction with ethyl acetate
5. washThe resulting organic layer was washed with a saturated aqueous solution of sodium chloride
6. dry with materialdried over magnesium sulfate
7. distillationthe solvent was distilled off under reduced pressure
8. customto give 2.9 g of a crude product
9. customThe obtained crude product
10. customwas purified with silica gel column chromatography (ethyl acetate/hexane=1/1-ethyl acetate alone)