Ethanol → HCID 12918690, compound

A 1-liter R.B. flask was equipped with a magnetic stirrer and charged with 104.13 g (0.400 mol) of 5-(2',4'-dichlorophenyl)-4-ketopentanoic acid dissolved in 250 ml of ethanol and 250 ml of toluene. To this solution was added 5 ml of concentrated sulfuric acid, and the reaction mixture was refluxed through a Soxhlet extractor containing 300 g of Type 3A molecular sieves for 24 hours. The mixture was cooled and 300 ml of the solvent removed on the Rotary Evaporator. The residue was taken up in 300 ml of ether and washed once with water. The mixture was extracted twice with 150 ml portions of 10% K2CO3 solution, then washed with saturated salt solution, and dried (MgSO4). The solvent was removed on the Rotary Evaporator, and the residue vacuum distilled. The product (52.97 g, 46% yield) was obtained as a slightly yellow viscous oil, b.p. 124°-165° C./0.10-0.30 mm.

1. customflask was equipped with a magnetic stirrer
2. temperaturethe reaction mixture was refluxed through a Soxhlet extractor
3. temperatureThe mixture was cooled
4. custom300 ml of the solvent removed on the Rotary Evaporator
5. washwashed once with water
6. extractionThe mixture was extracted twice with 150 ml portions of 10% K2CO3 solution
7. washwashed with saturated salt solution
8. dry with materialdried (MgSO4)
9. customThe solvent was removed on the Rotary Evaporator
10. distillationthe residue vacuum distilled

ORD record

ord-56857a727fdd43a0917c59202e2d4279

Source dataset

uspto-grants-1981_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04283348