Ethanol → Diethyl terephthalate

HRID 1089640ノート

反応式

HRID 1089640 の反応式
[O-:1]S([O-])(=O)=O.[Ca+2].[C:7](Cl)(=[O:17])[C:8]1[CH:16]=[CH:15][C:11]([C:12](Cl)=[O:13])=[CH:10][CH:9]=1.[CH2:19]([OH:21])[CH3:20].[C:22]1([CH3:28])C=CC=CC=1>>[C:7]([O:17][CH2:22][CH3:28])(=[O:1])[C:8]1[CH:16]=[CH:15][C:11]([C:12]([O:21][CH2:19][CH3:20])=[O:13])=[CH:10][CH:9]=1

参加物

5

反応物 4

HCID 702EthanolHCID 1140TolueneHCID 7488Terephthaloyl chlorideHCID 24497Calcium Sulfate

生成物 1

HCID 12483Diethyl terephthalate収率 86%

反応条件

温度
62.5 °C

実験手順

Into a 250 ml three-necked round bottom flask equipped with a mechanical stirrer and reflux condenser topped with a drying tube containing indicating Drierite® were added 100 ml of toluene and 40.6 grams (0.20) mole of terephthaloyl chloride. To this solution was added dropwise 18.4 grams (0.40 mole) of ethanol. The reaction solution was heated for two hours at 60-65° C. After this heating period IR analysis showed the complete disappearance of the acid chloride stretch at 1775 cm-1. The reaction solution was washed three times with 10% sodium bicarbonate solution and subsequently three times with distilled water. The product solution was dried over magnesium sulfate. After removal of the desiccant the toluene was removed by distillation. The residue crystallized on standing and amounted to 38 grams (86% yield) of diethyl terephthalate.

後処理

  1. customInto a 250 ml three-necked round bottom flask equipped with a mechanical stirrer
  2. temperaturereflux condenser
  3. customtopped with a drying tube
  4. additioncontaining
  5. waitAfter this heating period IR analysis showed
  6. washThe reaction solution was washed three times with 10% sodium bicarbonate solution and subsequently three times with distilled water
  7. dry with materialThe product solution was dried over magnesium sulfate
  8. customAfter removal of the desiccant the toluene
  9. customwas removed by distillation
  10. customThe residue crystallized on standing

出典と根拠

ORDレコード
ord-d50fc6799bde4f12b3c72c5e17efd06a
出典データセット
uspto-grants-1992_01
特許番号
US05078907

反応ノート

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