Potassium Iodide → HCID 23287876, Verbindung

The above benzonitrile (4.89 g, 26 mmol) was dissolved in methyl ethyl ketone (100 ml), and potassium carbonate (21.7 g, 157 mmol), potassium iodide (3.45 g, 52 mmol), and 5-(3-bromo-1-propylidene)-10,11-dihydro-5H-dibenzo[a,d]cycloheptene (8.18 g, 26 mmol), were added. The resulting mixture was stirred at reflux temperature for 18 h. After cooling to room temperature, ethyl acetate (200 ml) was added and the mixture was washed with water (2×150 ml), dried (MgSO4) and concentrated in vacuo. The residue was purified by flash chromatography on silica gel eluting first with a mixture of ethyl acetate and heptane (1:4), and then with a mixture of ethyl acetate and heptane (1:2). This afforded 5.60 g of the title compound as a solid.

1. temperatureat reflux temperature for 18 h
2. washthe mixture was washed with water (2×150 ml)
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. customThe residue was purified by flash chromatography on silica gel eluting first with a mixture of ethyl acetate and heptane (1:4)
6. additionwith a mixture of ethyl acetate and heptane (1:2)

ORD-Eintrag

ord-c5556c538f8b4880a083a5b7ead5a45d

Quelldatensatz

uspto-grants-1999_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05916889