Sulfuric Acid → Crotonic acid 2,2,2-trichloroethyl ester

HRID 249533

反応式

HRID 249533 の反応式
C(Cl)(Cl)(Cl)Cl.[C:6]([OH:11])(=[O:10])/[CH:7]=[CH:8]/[CH3:9].[Cl:12][C:13]([Cl:17])([Cl:16])[CH2:14]O.S(=O)(=O)(O)O>O>[Cl:12][C:13]([Cl:17])([Cl:16])[CH2:14][O:10][C:6](=[O:11])/[CH:7]=[CH:8]/[CH3:9]

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 5943Carbon TetrachlorideHCID 8259TrichloroethanolHCID 637090Crotonic Acid

生成物 1

HCID 15703159Crotonic acid 2,2,2-trichloroethyl ester収率 95%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

In 200 ml. carbon tetrachloride are dissolved 0.5 mole (43.07 g.) crotonic acid and the equimolar amount of 2,2,2-trichloroethanol, 1 ml. concentrated sulphuric acid is added thereto and the reaction mixture is heated under reflux on a water separator until the theoretical amount of water (9 ml.) has separated off. Subsequently, the organic phase is shaken out twice with, in each case, 100 ml. aqueous 2N sodium hydrogen carbonate solution and twice with, in each case, 50 ml. of water, the organic phase is then dried with anhydrous magnesium sulphate and the solvent is distilled off in a vacuum. There is finally obtained the desired product (i) in the form of a bright yellow oil in a yield of 95% of theory. C6H7O2Cl3. (217.4791).

後処理

  1. temperaturethe reaction mixture is heated
  2. customhas separated off
  3. dry with materialof water, the organic phase is then dried with anhydrous magnesium sulphate
  4. distillationthe solvent is distilled off in a vacuum

出典と根拠

ORDレコード
ord-f50bdbb835e34209bf80adf5c63d8046
出典データセット
uspto-grants-1993_05
特許番号
US05214195

関連ノート

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