三氟乙酸乙酯 → Butane-1,3-dione, 4,4,4-trifluoro-1-(4-imidazol-1-ylphenyl)-

温度

-78 °C

To a THF (5 mL) solution of 1,1,1,3,3,3-hexamethyldisilazane (0.178 g, 1.1 mmol) was added n-butyl lithum (1.6 M solution in hexane, 0.72 mL, 1.2 mmol) at 0° C. under nitrogen, and the mixture was stirred for 30 minutes, and cooled to −78° C. 4-(1-Imidazolyl)acetophenone (prepared according the method of M. A. Khan et. al., J. Chem. Soc. C., 1970, 85., 0.186 g, 1.0 mmol) was added to the mixture, and residue was stirred for 1 hour. Ethyl trifluoroacetate (0.17 g, 1.2 mmol) was added to the reaction mixture, the residue was warm to room temperature. The reaction mixture was poured into ice water and the whole was extracted with ethyl acetate (30 mL×2). The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The resulting solid was washed with small amount of ethyl acetate to give the title compound (0.163 g).

1. addition, 0.186 g, 1.0 mmol) was added to the mixture, and residue
2. stirringwas stirred for 1 hour
3. temperaturethe residue was warm to room temperature
4. extractionthe whole was extracted with ethyl acetate (30 mL×2)
5. washThe organic layer was washed with brine
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo
8. washThe resulting solid was washed with small amount of ethyl acetate

ORD记录

ord-3abc9b509f164373a025f10a80f8e6ad

来源数据集

uspto-grants-2005_09

DOI

10.6084/m9.figshare.5104873.v1

专利号

US06949536B2