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Ethylene Glycol → HCID 21999137、化合物

HRID 1375129
ノート
印刷プレビュー

反応式

HRID 1375129 の反応式
[CH3:1][CH:2]1[CH:7]([S:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)(=[O:10])=[O:9])[CH2:6][CH2:5][CH2:4][C:3]1=[O:17].[CH2:18](O)[CH2:19][OH:20].C(=O)(O)[O-].[Na+]>C1C=CC=CC=1>[CH2:18]1[CH2:19][O:20][C:3]2([CH2:4][CH2:5][CH2:6][CH:7]([S:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)(=[O:10])=[O:9])[CH:2]2[CH3:1])[O:17]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 3

HCID 174Ethylene GlycolHCID 516892Sodium BicarbonateHCID 21999124HCID 21999124、化合物

生成物 1

HCID 21999137HCID 21999137、化合物収率 95%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To a solution obtained by dissolving 1.4 g of 2-methyl-3-(phenylsulfonyl)-cyclohexan-1-one in 20 ml of benzene, were added 0.41 ml of 1,2-ethanediol and 0.1 g of anhydrous paratoluenesulfonic acid. The resulting mixture was heated under reflux for 4 hours. After the reaction, a 2M aqueous sodium bicarbonate solution was added and the resulting mixture was extracted with ethyl acetate three times. The combined organic layers were washed with saturated saline and dried over magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was recrystallized from ethyl ether, whereby 1,1-(ethylenedioxy)-2-methyl-3-(phenylsulfonyl)-cyclohexane was obtained in the form of white crystals. Yield: 95%, Melting point: 76 to 77° C.

後処理

  1. customTo a solution obtained
  2. temperatureThe resulting mixture was heated
  3. temperatureunder reflux for 4 hours
  4. customAfter the reaction
  5. extractionthe resulting mixture was extracted with ethyl acetate three times
  6. washThe combined organic layers were washed with saturated saline
  7. dry with materialdried over magnesium sulfate
  8. distillationThe solvent was distilled off under reduced pressure
  9. customThe residue was recrystallized from ethyl ether

出典と根拠

ORDレコード
ord-b278cc8be5274436adf69997e867dea6
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07166642B1

反応ノート

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