反応式
C[O:2][C:3]1([O:9][CH3:10])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.[CH3:11][C:12]([O:15]O)([CH3:14])[CH3:13]>C1(C)C=CC(S(O)(=O)=O)=CC=1.CS(C)=O>[CH3:10][O:9][C:3]1([O:2][O:15][C:12]([CH3:14])([CH3:13])[CH3:11])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1参加物
反応条件
- 温度
- 20 °C
実験手順
A mixed solution consisting of 16.4 g of dimethyl sulfoxide and 1.2 g of p-toluenesulfonic acid was kept at 20° C., and another mixed solution consisting of 28.9 g of cyclohexanone-dimethylacetal and 18.5 g of 1,1-dimethylethyl hydroperoxide was dropwise added to the former mixed solution. The resulting solution has an acid concentration of 0.1 mol/kg of the solution. The solution was stirred at 20° C. for 3 hours to complete the reaction. Then, 20 ml of petroleum ether was added to the solution, and the resulting solution was washed with 10 ml of water, then with 50 ml of a 5% NaOH aqueous solution, and further with 20 ml of water 3 times, and then dried by means of anhydrous sodium sulfate. The solvent was distilled off from the dried solution under vacuum to obtain 26.1 g (yield: 57%) of crude 1-methoxy-1-(1,1-dimethylethylperoxy)cyclohexane having a purity of 89%. The resulting crude peroxyketal was distilled at 40°-45° C. under a vacuum of 1 mmHg to obtain a purified peroxyketal having a purity of 99%.
後処理
- customwas kept at 20° C.
- additionwas dropwise added to the former mixed solution
- customthe reaction
- washthe resulting solution was washed with 10 ml of water
- dry with materialwith 50 ml of a 5% NaOH aqueous solution, and further with 20 ml of water 3 times, and then dried by means of anhydrous sodium sulfate
- distillationThe solvent was distilled off from the dried solution under vacuum
出典と根拠
- ORDレコード
- ord-c2c6505f94894b7f8d5baf77c0996f38
- 出典データセット
- uspto-grants-1991_04
- 特許番号
- US05004780
関連ノート
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