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Potassium Hydroxide → alpha,alpha-Dimethyl-3-thiopheneacetic acid

HRID 487531
ノート
印刷プレビュー

反応式

HRID 487531 の反応式
C[O:2][C:3](=[O:12])[C:4]([CH3:11])([C:6]1[CH:10]=[CH:9][S:8][CH:7]=1)[CH3:5].[OH-].[K+]>O.C(O)C>[CH3:11][C:4]([C:6]1[CH:10]=[CH:9][S:8][CH:7]=1)([CH3:5])[C:3]([OH:12])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 235103702-Methyl-2-thiophen-3-yl-propionic acid methyl ester

生成物 1

HCID 19092029alpha,alpha-Dimethyl-3-thiopheneacetic acid

試薬・触媒・溶媒 1

HCID 19096565Water ethanol溶媒

実験手順

The 2 -methyl-2-(3-thienyl)propionic acid methyl ester obtained in the foregoing Example 7 was added to a water:ethanol (1:4) solution (200 ml) of potassium hydroxide (18.5 g). Then the mixture was refluxed under heating for one hour and concentrated under reduced pressure, followed by a further addition of water thereto. Then the mixture was washed with dichloromethane (100 ml). The aqueous layer was acidified with diluted hydrochloric acid and the liberated carboxylic acid was extracted with dichloromethane (200 ml). The organic layer was dried over anhydrous magnesium sulfate, filtered and the solvent was removed by a water pump. The residue was recrystallized from hexane to obtain 2-methyl-2-(3-thienyl)propionic acid with mp. 78°-80.5° C.

後処理

  1. temperatureThen the mixture was refluxed
  2. temperatureunder heating for one hour
  3. concentrationconcentrated under reduced pressure
  4. additionfollowed by a further addition of water
  5. washThen the mixture was washed with dichloromethane (100 ml)
  6. extractionthe liberated carboxylic acid was extracted with dichloromethane (200 ml)
  7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. customthe solvent was removed by a water pump
  10. customThe residue was recrystallized from hexane

出典と根拠

ORDレコード
ord-cda11a45039f45178fa5016127fbdc67
出典データセット
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05296454

反応ノート

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