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1,1-Dimethoxycyclohexane → 1-Methoxy-1-[(2-methylbutan-2-yl)peroxy]cyclohexane

HRID 1084461
ノート
印刷プレビュー

反応式

HRID 1084461 の反応式
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:16]O)([CH3:15])[CH2:13][CH3:14]>C1(C)C=CC(S(O)(=O)=O)=CC=1.CS(C)=O>[CH3:10][O:9][C:3]1([O:2][O:16][C:12]([CH3:15])([CH3:11])[CH2:13][CH3:14])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 136161,1-DimethoxycyclohexaneHCID 76962tert-Amyl hydroperoxide

生成物 1

HCID 145730361-Methoxy-1-[(2-methylbutan-2-yl)peroxy]cyclohexane収率 77.4%

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒HCID 679Dimethyl Sulfoxide溶媒

実験手順

A mixed solution consisting of 15.9 g of dimethyl sulfoxide and 1.2 g of p-toluenesulfonic acid was kept at 20° C., into which was added dropwise another solution consisting of 29.1 g of cyclohexanone-dimethylacetal and 21.1 g of 1,1-dimethylpropyl hydroperoxide. The resulting solution had an acid concentration of 0.1 mol/kg of the solution. The solution was treated in the same manner as described in Example 1 to obtain 33.8 g (yield: 67%) of crude 1-methoxy-1-(1,1-dimethylpropylperoxy)cyclohexane having a purity of 86%. The resulting crude peroxyketal was distilled at 43°-45° C. under a vacuum of 0.1 mmHg to obtain a purified peroxyketal having a purity of 98%.

後処理

  1. customwas kept at 20° C., into which
  2. additionwas added dropwise another solution
  3. additionThe solution was treated in the same manner

出典と根拠

ORDレコード
ord-894a0d2ba051497b83f47d4f19a68f62
出典データセット
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05004780

反応ノート

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