Hydrochloric Acid → 2-Phenylisobutyric acid
Reaction equation
[CH2:1]([C:8]#N)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-:10].[K+].S(OC)([O:15][CH3:16])(=O)=O.Cl.[CH3:20]S(C)=O>>[CH3:20][C:1]([CH3:8])([C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:16]([OH:15])=[O:10]Participants
Procedure
Benzyl cyanide (0.5 kg), potassium hydroxide (1.4 kg) and DMSO (2.5 ltr) were initially charged to a reactor and dimethyl sulphate (1.20 kg) was slowly added thereto over a period of one hour. The mixture was stirred for 3-4 hours at room temperature. The mass was slowly quenched in water with stirring. The pH was adjusted to 1-2 with conc HCl. The solution was filtered, the solids washed with water and the resulting material was dried under vacuum in an oven. The resulting product was suspended in water (3.0 ltr), sodium hydroxide (0.5 kg) added thereto and the mixture refluxed for 6 hours. After completion of the reaction, the reaction mass was cooled to room temperature and acidified with HCl to pH 2-3. The resulting precipitated material was filtered, washed with water and dried to obtain the title product.
Workup
- customThe mass was slowly quenched in water
- stirringwith stirring
- filtrationThe solution was filtered
- washthe solids washed with water
- customthe resulting material was dried under vacuum in an oven
- additionsodium hydroxide (0.5 kg) added
- temperaturethe mixture refluxed for 6 hours
- customAfter completion of the reaction
- temperaturethe reaction mass was cooled to room temperature
- customThe resulting precipitated material
- filtrationwas filtered
- washwashed with water
- customdried
Sources & evidence
- ORD record
- ord-b6ec1efac6064ea4b3b78ca851885463
- Source dataset
- uspto-grants-2012_08
- Patent number
- US08247434B2
Reaction notes
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