Benzaldehyde, 4-(phenylmethoxy)- → 4-Benzyloxy-benzaldehyde oxime

HRID 77737노트

반응식

HRID 77737 반응식
[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=O)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:17][OH:18].Cl.C([O-])(=O)C.[Na+]>C(O)C.O>[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=[N:17][OH:18])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 78109Benzaldehyde, 4-(phenylmethoxy)-HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium Acetate

생성물 1

HCID 7633594-Benzyloxy-benzaldehyde oxime

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 962Water용매2회

실험 절차

4.24 g of 4-benzyloxy benzaldehyde (20 mmol) was dissolved in a 0.2M mixed solution of ethanol and water (3:1,100 ml), followed by stirring. 2.78 g of NH2OH—HCl (40 mmol) and 2.46 g of sodium acetate(30 mmol) were added thereto, and stirred at room temperature for about 30 minutes. Subsequently, the completion of the reaction was confirmed by liquid chromatography, and water and ethanol were removed by distillation under reduced pressure to obtain a pale yellow solid compound. The pale yellow solid compound was extracted three times with water and ethyl acetate, an organic solvent layer was dried under reduced pressure to obtain a crude product, and the crude product was then purified with a hexane/ethylacetate solution (10:1) to obtain a white solid compound. The obtained solid compound was subjected to subsequent reactions without additional purification.

후처리

  1. stirringstirred at room temperature for about 30 minutes
  2. customwere removed by distillation under reduced pressure
  3. customto obtain a pale yellow solid compound
  4. extractionThe pale yellow solid compound was extracted three times with water and ethyl acetate
  5. customan organic solvent layer was dried under reduced pressure

출처 및 근거

ORD 기록
ord-3f0ce4815c904f29a068b340a3954c8a
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841335B2

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