Hydroxyamine hydrochloride → 3-(alpha-Hydroxyiminopropyl)-5-[(2,4-dichlorophenoxy)methyl]-1,2,4-oxadiazole

HRID 4898노트

반응식

HRID 4898 반응식
[CH2:1]([C:3]([C:5]1[N:9]=[C:8]([CH2:10][O:11][C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:13]=2[Cl:19])[O:7][N:6]=1)=O)[CH3:2].Cl.[OH:21][NH2:22]>CO>[OH:21][N:22]=[C:3]([C:5]1[N:9]=[C:8]([CH2:10][O:11][C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:13]=2[Cl:19])[O:7][N:6]=1)[CH2:1][CH3:2]

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 197971233-Ethylcarbonyl-5-[(2,4-dichlorophenoxy)methyl]-1,2,4-oxadiazole

생성물 1

HCID 1363314963-(alpha-Hydroxyiminopropyl)-5-[(2,4-dichlorophenoxy)methyl]-1,2,4-oxadiazole수율 85%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

0.9 g of 3-ethylcarbonyl-5-[(2,4-dichlorophenoxy)methyl]-1,2,4-oxadiazole and 0.21 g of hydroxyamine hydrochloride were added to 10 ml of methanol. The mixture was heated to reflux for 4 hours. After evaporation of methanol, water was added to the residue. The aqueous solution was extracted with ethylacetate. After evaporation of ethylacetate, the residue was purified by column chromatography(benzene:ether=1.1) to provide 0.80 g of the desired product(yield: 85.0%).

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 4 hours
  3. customAfter evaporation of methanol, water
  4. additionwas added to the residue
  5. extractionThe aqueous solution was extracted with ethylacetate
  6. customAfter evaporation of ethylacetate
  7. customthe residue was purified by column chromatography(benzene:ether=1.1)

출처 및 근거

ORD 기록
ord-ee847813e8e14c88ba9cb5b8597ec847
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05242890

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