Potassium Carbonate → 1,2,3-Trichloro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzene

Temperatur

80 °C

A mixture of 3,4,5-trichlorophenylboronic acid (3.376 g, 15 mmol), 2-bromo-3,3,3-trifluoroprop-1-ene (4.02 g, 23 mmol), K2CO3 (4.15 g, 30 mmol) and Pd(PPh3)2Cl2 (4.15 g, 30 mmol) in THF (16 mL) and H2O (8 mL) was heated at 80° C. in a sealed tube for 4 h. The mixture was cooled to rt and partitioned between EA (50 mL) and H2O (50 mL). The aqueous layer was extracted with EA (50 mL) and the combined organic layers were dried over anhydrous Na2SO4. The solvent was removed under reduced pressure and the crude product was purified by column chromatography on silica gel to give the crude desired product (3.7 g; 90% yield) as a pale yellow solid.

1. temperatureThe mixture was cooled to rt
2. custompartitioned between EA (50 mL) and H2O (50 mL)
3. extractionThe aqueous layer was extracted with EA (50 mL)
4. dry with materialthe combined organic layers were dried over anhydrous Na2SO4
5. customThe solvent was removed under reduced pressure
6. customthe crude product was purified by column chromatography on silica gel

ORD-Eintrag

ord-c16bde3d71104befa489ca074c9ea321

Quelldatensatz

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08853186B2