Acetone → 2-Chlorobenzylideneacetone

Temperature

0 °C

A mixture of 2-chlorobenzaldehyde (25.0 g, 178 mmol), acetone (40 ml) and water (20 ml) was cooled to 0° C., followed by adding dropwise thereto a 5% aqueous sodium hydroxide solution (7 ml), and the resulting mixture was stirred at room temperature for 4 hours. The reaction mixture was adjusted to pH 1 with 1N hydrochloric acid and extracted with ethyl acetate. The extract solution was washed with water and a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure and the resulting residue was purified by a silica gel column chromatography to obtain 13.2 g of 1-(2-chlorophenyl)-1-buten-3-one.

1. additionby adding dropwise
2. extractionextracted with ethyl acetate
3. washThe extract solution was washed with water
4. dry with materiala saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate
5. distillationThe solvent was distilled off under reduced pressure
6. customthe resulting residue was purified by a silica gel column chromatography

ORD record

ord-93a385348e09439ea2ecddc349d1383c

Source dataset

uspto-grants-2002_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06369110B1