Hydroxyamine hydrochloride → 3-Chloro-4-methylbenzaldoxime

HRID 1880232노트

반응식

HRID 1880232 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[CH3:10])[CH:5]=O.Cl.[NH2:12][OH:13]>CO.O.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[CH3:10])[CH:5]=[N:12][OH:13]

참가 물질

6

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 124230853-Chloro-4-methylbenzaldehyde

생성물 1

HCID 730143123-Chloro-4-methylbenzaldoxime

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 5.0 g of 3-chloro-4-methylbenzaldehyde in 40 mL of methanol and 30 mL of water, 4.7 g of hydroxylamine hydrochloride was added and the resultant mixture was stirred at room temperature for 2 hours. After the completion of the reaction, the reaction mixture was diluted with 70 mL of ethyl acetate and the diluted reaction mixture was washed with water (30 mL×1) and then dehydrated and dried over saturated saline and anhydrous sodium sulfate in this order, followed by distilling off the solvent under reduced pressure to obtain 5.1 g of the objective substance as a white crystal. This crystal was used in the next process as it was without being further purified.

후처리

  1. customAfter the completion of the reaction
  2. customthe diluted reaction mixture
  3. washwas washed with water (30 mL×1)
  4. dry with materialdried over saturated saline and anhydrous sodium sulfate in this order
  5. distillationby distilling off the solvent under reduced pressure
  6. customto obtain 5.1 g of the objective substance as a white crystal

출처 및 근거

ORD 기록
ord-a1e18b6c285f4eaca6ba2e6163199e31
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08318757B2

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