Sodium Carbonate → 1,3-Bis[4-[4-(4-isopropoxy-3,5-dimethoxyphenyl)benzoyl]-1-piperazinyl]propane

Temperatur

80 °C

Under nitrogen were added 2.40 mL (48 mmol) of a 2 mol/L aqueous sodium carbonate solution and 729.9 mg (0.632 mmol) of tetrakis(triphenylphosphine)palladium (0) to a solution of 4.50 g (7.79 mmol) of 1,3-bis[4-(4-bromobenzoyl)-1-piperazinyl]propane and 4.50 g (18.7 mmol) of 4-isopropoxy-3,5-dimethoxyphenylboronic acid in ethanol-toluene (15 mL -60 mL), and the mixture was stirred for 3 hours at 80° C. The reaction mixture was concentrated under reduced pressure to remove the organic solvents. Water (15 mL) was added to the residue and the mixture was extracted with chloroform (100 mL, 3×30 mL). The organic layers were combined, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by chromatography on silica gel to give 5.93 g of 1,3-bis[4-[4-(4-isopropoxy-3,5-dimethoxyphenyl)benzoyl]-1-piperazinyl]propane as a colorless oil (yield 94%).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. customto remove the organic solvents
3. additionWater (15 mL) was added to the residue
4. extractionthe mixture was extracted with chloroform (100 mL, 3×30 mL)
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by chromatography on silica gel

ORD-Eintrag

ord-02ca2cf3049d4966a43346bf430d9afb

Quelldatensatz

uspto-grants-2004_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06787653B2