Aluminum isopropoxide → 3-(1-Hydroxybutyl)-5-[(2,4-dichlorophenoxy)methyl]-1,2,4-oxadiazole

HRID 4899

反応式

HRID 4899 の反応式
[CH2:1]([C:4]([C:6]1[N:10]=[C:9]([CH2:11][O:12][C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=2[Cl:20])[O:8][N:7]=1)=[O:5])[CH2:2][CH3:3].CC(C)[O-].[Al+3].CC(C)[O-].CC(C)[O-]>C(O)(C)C>[OH:5][CH:4]([C:6]1[N:10]=[C:9]([CH2:11][O:12][C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=2[Cl:20])[O:8][N:7]=1)[CH2:1][CH2:2][CH3:3]

参加物

4

反応物 2

HCID 11143Aluminum isopropoxideHCID 197971373-Propylcarbonyl-5-[(2,4-dichlorophenoxy)methyl]-1,2,4-oxadiazole

生成物 1

HCID 197971383-(1-Hydroxybutyl)-5-[(2,4-dichlorophenoxy)methyl]-1,2,4-oxadiazole収率 54%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

0.316 g of 3-propylcarbonyl-5-[(2,4-dichlorophenoxy)methyl]-1,2,4-oxadiazole and 0.20 g of aluminum isopropoxide were added to 10 ml of isopropanol. The mixture was heated to reflux for 48 hours. After evaporation of isopropanol, water was added to the residue. The aqueous solution was extracted with ethylacetate. After evaporation of ethylacetate, the residue was purified by column chromatography(hexane: ethylacetate=3:2) to provide 0.17 g of the desired product(yield: 54.0%).

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 48 hours
  3. customAfter evaporation of isopropanol, 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(hexane: ethylacetate=3:2)

出典と根拠

ORDレコード
ord-71d372ee817748b9b806f8449f71356b
出典データセット
uspto-grants-1993_09
特許番号
US05242890

関連ノート

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