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Hydrazine hydrate (1:1) → HCID 19790226, 화합물

HRID 569354
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HRID 569354 반응식
C1(=O)[N:5]([O:6][CH2:7]/[CH:8]=[CH:9]/[C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])C(=O)C2=CC=CC=C12.O.NN>C(Cl)Cl.CO>[NH2:5][O:6][CH2:7]/[CH:8]=[CH:9]/[C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11]
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참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 19790246HCID 19790246, 화합물

생성물 1

HCID 19790226HCID 19790226, 화합물수율 96.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

To a solution of tert-butyl 4-phthalimidooxycrotonate (20.0 g) in methylene chloride (140 ml) was added a solution of hydrazine monohydrate (5.0 g) in methanol (10 ml) with stirring, and the stirring was continued at ambient temperature for 15 minutes. The insoluble substance was collected by filtration and washed with methylene chloride. The washings and the filtrate were combined and then extracted three times with 5% hydrochloric acid. After the combined extracts were washed with diethyl ether, thereto was added methylene chloride, followed by adjusting to pH 7.5 with 28% aqueous ammonium hydroxide. The separated methylene chloride solution was washed with a saturated aqueous sodium chloride and then dried over magnesium sulfate. Removal of the solvent gave an oil of tertbutyl 4-aminooxycrotonate (11.03 g).

후처리

  1. filtrationThe insoluble substance was collected by filtration
  2. washwashed with methylene chloride
  3. extractionextracted three times with 5% hydrochloric acid
  4. washAfter the combined extracts were washed with diethyl ether
  5. additionwas added methylene chloride
  6. washThe separated methylene chloride solution was washed with a saturated aqueous sodium chloride
  7. dry with materialdried over magnesium sulfate
  8. customRemoval of the solvent

출처 및 근거

ORD 기록
ord-c80fe72b607b44a1b461ce43cc13b272
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04731443

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