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

HRID 487531노트

반응식

HRID 487531 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 19096565Water ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cda11a45039f45178fa5016127fbdc67
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05296454

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