Reaction equation
[CH3:1][C:2]([CH3:4])=O.[CH2:5]([O:8][CH2:9][CH:10]([OH:13])[CH2:11][OH:12])[CH:6]=[CH2:7].S(=O)(=O)(O)O>C1(C)C=CC=CC=1>[CH2:5]([O:8][CH2:9][CH:10]1[CH2:11][O:12][C:2]([CH3:4])([CH3:1])[O:13]1)[CH:6]=[CH2:7]Participants
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
The 4-allyloxymethyl-2,2-dimethyl-1,3-dioxolane was prepared by mixing acetone, 225 parts, 3-allyloxy-1,2-propanediol, 195 parts and toluene, 480 parts in a flask fitted with a magnetic stirring bar and a water trap mounted with a reflux condenser. Concentrated sulfuric acid, 4 parts, was added to the flask and the mixture was heated to reflux. The first 170 parts of distillate were removed via the water trap, after which reflux was conducted and water was collected in the water trap. After 13 hours the reaction mixture was cooled, neutralized with aqueous sodium bicarbonate, distilled to remove water and toluene and then distilled under vacuum to give 161 parts of 4-allyloxymethyl-2,2-dimethyl-1,3-dioxolane having a boiling point of 57° to 58° at 4.5 Torr.
Workup
- customThe 4-allyloxymethyl-2,2-dimethyl-1,3-dioxolane was prepared
- customfitted with a magnetic stirring bar and a water trap
- custommounted with a reflux condenser
- temperaturethe mixture was heated to reflux
- customThe first 170 parts of distillate were removed via the water trap
- temperatureafter which reflux
- customwater was collected in the water trap
- temperatureAfter 13 hours the reaction mixture was cooled
- distillationdistilled
- customto remove water and toluene
- distillationdistilled under vacuum
Sources & evidence
- ORD record
- ord-0f33f28672da42469efd880561463591
- Source dataset
- uspto-grants-1990_03
- Patent number
- US04908228
Linked notes
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