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

HRID 4898ノート

反応式

HRID 4898 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-ee847813e8e14c88ba9cb5b8597ec847
出典データセット
uspto-grants-1993_09
特許番号
US05242890

反応ノート

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