3-Buten-2-one, 4-butoxy-1,1,1-trifluoro-, (3E)- synthesis

Yield: 0.87 g

Reaction Conditions:

with pyridine;methanesulfonyl chloride;triethylamine in dichloromethane at 20; for 48 h;Time;

Steps:

19 Synthesis of (E) -4-butoxy-1,1,1-trifluoro-3-buten-2-one
To a mixed solution of 0.50 g (4.39 mmol) of trifluoroacetic acid and 9 ml of dichloromethane were added 0.35 g (4.39 mmol) of pyridine, 0.53 g (5.26 mmol) of triethylamine, n-butyl vinyl ether 44 g (4.38 mmol) and 0.50 g (4.38 mmol) methanesulfonyl chloride were added. After stirring at room temperature for 48 hours, 10 ml of ice water was added to the reaction mixture, and the mixture was extracted with 10 ml of chloroform. The obtained organic layer was washed with 10 ml of 1 mol / L hydrochloric acid and 10 ml of a saturated sodium hydrogencarbonate aqueous solution, then dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 0.87 g of the objective compound as a yellow oil Obtained.

References:

NISSAN CHEMICAL INDUSTRIES LIMITED;NAKAYA, YOSHIHIKO;TANIMA, DAISUKE;INABA, MASAMITSU;MIYAKADO, YUUKI;FURUHASHI, TAKAMASA;MAEDA, KAZUSHIGE JP2017/25054, 2017, A Location in patent:Paragraph 0231; 0232