Potassium Hydroxide → HCID 54158494, compound
Reaction equation
[OH-].[K+].[CH3:3][C:4]([O:8][OH:9])([CH:6]=[CH2:7])[CH3:5].[C:10](Cl)(=[O:15])[C:11]([CH3:14])([CH3:13])[CH3:12]>O>[C:10]([O:9][O:8][C:4]([CH3:5])([CH:6]=[CH2:7])[CH3:3])(=[O:15])[C:11]([CH3:14])([CH3:13])[CH3:12]Participants
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
To a stirred mixture cooled at 10° C. of 10 g of demineralized water, 17.3 g of a 45% by weight-potassium hydroxide solution in water (0.139 moles) and 12.9 g of 2-methyl-3-buten-2-yl hydroperoxide (0.120 moles) there were added over a period of 25 minutes 14.5 g of pivaloyl chloride (0.120 moles); the temperature of the reaction mixture was kept at 10°-12° C. Stirring was continued for 1 hour, after which the organic layer was isolated. It was washed successively with an aqueous solution of 10% by weight-KOH (15 min, 10° C.), an aqueous bisulphite/acetate buffer (20 min., 10° C.) and a dilute solution of sodium bicarbonate in water (2x). Finally, the organic layer was dried with MgSO4 and the product was isolated by filtration. There were obtained 17.3 g of colourless oil containing 97.7% of peroxy ester, which corresponds to a yield of 75.6 %. The identity of the product was confirmed by IR and NMR spectroscopy (1H and 13C).
Workup
- customwas kept at 10°-12° C
- customafter which the organic layer was isolated
- washIt was washed successively with an aqueous solution of 10% by weight-KOH (15 min, 10° C.)
- customan aqueous bisulphite/acetate buffer (20 min., 10° C.)
- dry with materialFinally, the organic layer was dried with MgSO4
- customthe product was isolated by filtration
Sources & evidence
- ORD record
- ord-e2ed8aad7de144e282a95d1179189e8a
- Source dataset
- uspto-grants-1987_11
- Patent number
- US04705888
Reaction notes
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