Hydroxyamine hydrochloride → 4-Phenoxyphenoxyacetone oxime

HRID 35279ノート

反応式

HRID 35279 の反応式
Cl.[NH2:2][OH:3].C([O-])(=O)C.[Na+].[O:9]([C:16]1[CH:26]=[CH:25][C:19]([O:20][CH2:21][C:22](=O)[CH3:23])=[CH:18][CH:17]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>O.C(O)C>[O:9]([C:16]1[CH:26]=[CH:25][C:19]([O:20][CH2:21][C:22](=[N:2][OH:3])[CH3:23])=[CH:18][CH:17]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

6

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 137717024-Phenoxyphenoxyacetone

生成物 1

HCID 867423654-Phenoxyphenoxyacetone oxime

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Over about 1 hour, a solution of 22 g of hydroxylamine hydrochloride and 26 g of anhydrous sodium acetate in 110 ml of water is added dropwise at room temperature to a solution of 64 g of 4-phenoxyphenoxyacetone in 260 ml of ethanol. After the slightly exothermic reaction has subsided, the mixture is stirred for a further 3.5 hours at reflux temperature. Subsequently, the ethanol is distilled off from the reaction mixture by rotary evaporation, the aqueous residue is extracted three times with a 2:1 mixture of ether and hexane, the combined organic phases are washed with water and with 10% sodium bicarbonate solution and then dried over sodium sulfate. The solvent is then distilled off. Recrystallisation from a mixture of diethyl ether and pentane affords 4-phenoxyphenoxyacetone oxime with a melting point of 59°-61° C.

後処理

  1. customAfter the slightly exothermic reaction
  2. temperatureat reflux temperature
  3. distillationSubsequently, the ethanol is distilled off from the reaction mixture by rotary evaporation
  4. extractionthe aqueous residue is extracted three times
  5. additionwith a 2:1 mixture of ether and hexane
  6. washthe combined organic phases are washed with water and with 10% sodium bicarbonate solution
  7. dry with materialdried over sodium sulfate
  8. distillationThe solvent is then distilled off
  9. customRecrystallisation
  10. additionfrom a mixture of diethyl ether and pentane

出典と根拠

ORDレコード
ord-f4cb6a7e299043e7b3155f8a624b2916
出典データセット
uspto-grants-1988_08
特許番号
US04766152

反応ノート

読み込み中…