Ethyl trifluoroacetate → 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, 1.2mmol) 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 tothe reaction mixture, the residure 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. customtothe reaction mixture
4. temperaturethe residure was warm to room temperature
5. extractionthe whole was extracted with ethyl acetate (30 mL×2)
6. washThe organic layer was washed with brine
7. dry with materialdried over Na2SO4
8. concentrationconcentrated in vacuo
9. washThe resulting solid was washed with small amount of ethyl acetate

ORDレコード

ord-014edeebc2ec4087a1b941830e15dd7f

出典データセット

uspto-grants-2003_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06608095B2