反应详情

温度

0 °C

5 g (22.7 mmol) of 4-allyl-1-ethoxymethoxy-2-ethylbenzene are dissolved in 100 ml of anhydrous THF, and the medium is cooled to 0° C. 6.6 g (27 mmol) of 9-BBN are added, and the medium is brought to room temperature and then stirred for 12 hours. A solution of 7.8 g (22.6 mmol) of dimethyl 4-trifluoromethanesulphonyloxyphthalate in 100 ml of DMF is added, as well as 6.2 g (44.8 mmol) of potassium carbonate. The reaction medium is degassed with a nitrogen stream, and then 930 mg (1.1 mmol) of dichloropalladium diphosphinoferrocene are added. The medium is heated at 50° C. for 3 hours, and then poured into an ammonium chloride solution and extracted with ethyl acetate. The residue obtained after drying and concentration is purified by chromatography on a silica column (eluent heptane, and then heptane 85/ethyl acetate 15). A yellow oil is obtained (m=6.9 g, y=73%).

1. customis brought to room temperature
2. customThe reaction medium is degassed with a nitrogen stream
3. temperatureThe medium is heated at 50° C. for 3 hours
4. extractionextracted with ethyl acetate
5. customThe residue obtained
6. customafter drying
7. concentrationconcentration
8. customis purified by chromatography on a silica column (eluent heptane
9. customA yellow oil is obtained (m=6.9 g, y=73%)