Hydrochloric Acid → alpha,3-Dichlorobenzaldoxime

HRID 332316노트

반응식

HRID 332316 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)/[CH:5]=[N:6]\[OH:7].[ClH:11].OS([O-])(=O)=O.OS(O[O-])(=O)=O.OS(O[O-])(=O)=O.[O-]S([O-])(=O)=O.[K+].[K+].[K+].[K+].[K+]>CN(C=O)C>[OH:7]/[N:6]=[C:5](\[Cl:11])/[C:4]1[CH:8]=[CH:9][CH:10]=[C:2]([Cl:1])[CH:3]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 5372364Benzaldehyde, m-chloro-, oxime, (Z)-HCID 15793144Potassium caroate

생성물 1

HCID 10943262alpha,3-Dichlorobenzaldoxime수율 100%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of (E)- and/or (Z)-3-chloro-benzaldehyde oxime (54 g, 347 mmol) in DMF (800 mL) was added HCl (conc., 17 mL) and the mixture cooled to room temperature. Then potassium monopersulfate triple salt (247 g, 400 mmol) and the reaction mixture was stirred at room temperature for 1 h. The mixture was then poured onto ice-water, and extracted with ethyl acetate. The combined organic layers were then washed with water and brine, dried over sodium sulfate and evaporated to afford the title compound (66 g, 100%) which was obtained as a white solid. Mp: 58-60° C.

후처리

  1. additionThe mixture was then poured onto ice-water
  2. extractionextracted with ethyl acetate
  3. washThe combined organic layers were then washed with water and brine
  4. dry with materialdried over sodium sulfate
  5. customevaporated

출처 및 근거

ORD 기록
ord-3d2bd0d6e9a44b65a0dc97829dd472a4
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877783B2

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