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Hydrazine hydrate (1:1) → Methyl alpha-methylthio-alpha-(3-chloro-4-aminophenyl)propionate

HRID 1277772
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반응식

HRID 1277772 반응식
[CH3:1][S:2][C:3]([C:9]1[CH:14]=[CH:13][C:12]([N:15]2C(=O)C3=CC=CC=C3C2=O)=[C:11]([Cl:26])[CH:10]=1)([CH3:8])[C:4]([O:6][CH3:7])=[O:5].O.NN>CO>[CH3:1][S:2][C:3]([C:9]1[CH:14]=[CH:13][C:12]([NH2:15])=[C:11]([Cl:26])[CH:10]=1)([CH3:8])[C:4]([O:6][CH3:7])=[O:5]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 12819454Methyl alpha-methylthio-alpha-(3-chloro-4-phthalimidophenyl)propionate

생성물 1

HCID 12917666Methyl alpha-methylthio-alpha-(3-chloro-4-aminophenyl)propionate수율 92%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Methyl α-methylthio-α-(3-chloro-4-phthalimido-phenyl)propionate was suspended in 7 ml of methanol, and 97 mg of hydrazine hydrate was added. The mixture was stirred at room temperature, and then heated under reflux for 1 hour. The mixture was concentrated under reduced pressure, and an aqueous solution of ammonium chloride and methylene chloride were added. The organic layer was separated, and dried over anhydrous sodium sulfate. Concentration under reduced pressure yielded 231 mg of methyl α-methylthio-α-(3-chloro-4-aminophenyl)propionate as a pale yellow oil. Yield 92%.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 1 hour
  3. concentrationThe mixture was concentrated under reduced pressure
  4. additionan aqueous solution of ammonium chloride and methylene chloride were added
  5. customThe organic layer was separated
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationConcentration under reduced pressure

출처 및 근거

ORD 기록
ord-4e85efa006ac4317bf37c622da25fff5
출처 데이터셋
uspto-grants-1981_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04278802

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