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2-Ethylhexanol → di(2-ethylhexyl) (2Z)-2-methyl-2-butenedioate

HRID 1397647
ノート
印刷プレビュー

反応式

HRID 1397647 の反応式
[C:1]1(=[O:8])[O:7][C:5](=[O:6])[CH:4]=[C:2]1[CH3:3].[CH2:9]([CH:11]([CH2:14][CH2:15][CH2:16][CH3:17])[CH2:12][OH:13])[CH3:10].[C:18]1([CH3:27])[CH:23]=[CH:22][C:21](S(=O)=O)=[CH:20][CH:19]=1.[CH2:28](OC(=O)C)C>>[CH2:9]([CH:11]([CH2:14][CH2:15][CH2:16][CH3:17])[CH2:12][O:13][C:1](=[O:8])/[C:2](=[CH:4]\[C:5]([O:7][CH2:28][CH:21]([CH2:20][CH3:19])[CH2:22][CH2:23][CH2:18][CH3:27])=[O:6])/[CH3:3])[CH3:10]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 77202-EthylhexanolHCID 8857Ethyl AcetateHCID 12012Citraconic AnhydridesHCID 178427284HCID 178427284、化合物

生成物 1

HCID 86683840di(2-ethylhexyl) (2Z)-2-methyl-2-butenedioate

反応条件

温度
160 °C

実験手順

10 ml of citraconic anhydride (CAS no 616-02-4) and 53 ml of 2-ethyl-hexanol (CAS no 104-76-7) and 0.3 g of p-toluenesulfonic acid monohydride (CAS n 6192-52-5) were mixed in a glass flask at room temperature. The mixture was heated to 160° C., and maintained at that temperature under stirring overnight. Thereafter the mixture was cooled and diluted with 50 ml of ethylacetate, and washed twice with 100 ml of 10% NaHCO3 solution and twice with 50 ml of water, and dried with MgSO4, and filtered. Final purification of citraconate was done by vacuum distillation.

後処理

  1. temperaturemaintained at that temperature
  2. temperatureThereafter the mixture was cooled
  3. washwashed twice with 100 ml of 10% NaHCO3 solution and twice with 50 ml of water
  4. dry with materialdried with MgSO4
  5. filtrationfiltered
  6. customFinal purification of citraconate
  7. distillationwas done by vacuum distillation

出典と根拠

ORDレコード
ord-534eb1affc51422fb62c0e8d6f83d387
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08901261B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート