Potassium Cyanide → HCID 19898197, compound

A solution of 3,4-dichlorobenzoyl chloride (2.1 g) in dry acetonitrile (10 ml) was added at ambient temperature to a stirred solution of piperidine-2,4-dione (1.13 g) and dry triethylamine (1.31 g) in dry acetonitrile (50 ml) and the mixture stirred at ambient temperature for 18 hours. Potassium cyanide (0.06 g) dry triethylamine (3.1 g) and tris-(3,6-dioxaheptyl)amine (0.5 ml) were added successively and the mixture stirred at ambient temperature for 24 hours. The mixture was evaporated under reduced pressure and the residue dissolved in dichloromethane (50 ml). The dichloromethane solution was washed successively with 2N hydrochloric acid (2×30 ml) and water (3×30 ml), dried over magnesium sulphate and evaporated under reduced pressure to give a brown solid which was purified by column chromatography to give 3-(3,4-dichlorobenzoyl)piperidine-2,4-dione (0.37 g) mp 171.5°-174.5° C., as a cream crystalline solid.

1. stirringthe mixture stirred at ambient temperature for 24 hours
2. customThe mixture was evaporated under reduced pressure
3. dissolutionthe residue dissolved in dichloromethane (50 ml)
4. washThe dichloromethane solution was washed successively with 2N hydrochloric acid (2×30 ml) and water (3×30 ml)
5. dry with materialdried over magnesium sulphate
6. customevaporated under reduced pressure
7. customto give a brown solid which
8. customwas purified by column chromatography

ORD record

ord-ad4aa41a710841e392d39690852dadc4

Source dataset

uspto-grants-1992_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05114461