Acetic Acid → N-[4-(4-aminophenyl)butanoyl]thiazolidine

HRID 1614561노트

반응식

HRID 1614561 반응식
C(O)(=O)C.[N+:5]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][CH2:16][C:17]([N:19]2[CH2:23][CH2:22][S:21][CH2:20]2)=[O:18])=[CH:10][CH:9]=1)([O-])=O>[Zn].O>[NH2:5][C:8]1[CH:9]=[CH:10][C:11]([CH2:14][CH2:15][CH2:16][C:17]([N:19]2[CH2:23][CH2:22][S:21][CH2:20]2)=[O:18])=[CH:12][CH:13]=1

참가 물질

5

반응물 2

HCID 176Acetic AcidHCID 14822253N-[4-(4-nitrophenyl)butanoyl]thiazolidine

생성물 1

HCID 14822257N-[4-(4-aminophenyl)butanoyl]thiazolidine수율 67%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 962Water용매

실험 절차

To a mixture of 9 ml of acetic acid, 6 ml of water, and 1.0 g of zinc powder was gradually added 2 mmol of N-[4-(4-nitrophenyl)butanoyl]thiazolidine at room temperature in small portions with stirring. After the addition, the mixture was stirred for 2 hours at the same temperature to complete the reaction. Zinc powder was removed by filtration. The filtrate was weakly alkalinized with 10% sodium hydroxide and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by column chromatography on silica gel to obtain 335 mg of colorless crystals of N-[4-(4-aminophenyl)butanoyl]thiazolidine (yield: 67%).

후처리

  1. customat room temperature
  2. additionAfter the addition
  3. stirringthe mixture was stirred for 2 hours at the same temperature
  4. customthe reaction
  5. customZinc powder was removed by filtration
  6. extractionextracted with ethyl acetate
  7. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  8. customThe solvent was evaporated under reduced pressure
  9. customthe residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-9efac4512e8a479e9e6896a4a9deeb53
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05198450

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