Hydroxyamine hydrochloride → HCID 86742368、化合物

HRID 35281ノート

反応式

HRID 35281 の反応式
Cl.[NH2:2][OH:3].[O:4]([C:11]1[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][C:19](=O)[CH3:20])=[CH:13][CH:12]=1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1>O.[OH-].[Na+].C(O)C>[O:4]([C:11]1[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][C:19](=[N:2][OH:3])[CH3:20])=[CH:13][CH:12]=1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

参加物

6

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 212962814-(4-Phenoxyphenyl)-2-butanone

生成物 1

HCID 86742368HCID 86742368、化合物

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

Over about 30 minutes, a freshly prepared solution of 15.3 g (0.22 mole) of hydroxylamine hydrochloride in 100 ml of water and 200 ml of 1N sodium hydroxide solution is added dropwise at room temperature to a solution of 48 g (0.2 mole) of 4-(4-phenoxyphenyl)-2-butanone*) in 500 ml of ethanol. Subsequently, the mixture is heated for 1.5 hours at reflux temperature and then stirred for 16 hours at room temperature. The ethanol is distilled off in a water jet vacuum and the residue is extracted repeatedly with ether. The combined ethereal phases are washed repeatedly with water and dried over sodium sulfate and the ther is distilled off entirely. The crude oxime is chromatographed over silica gel (eluant: a 1:1 mixture of diethyl ether and n-hexane). The resultant 4-(4-phenoxyphenyl)-2-butanone oxime melts at 80°-82° C. after recrystallisation in a mixture of diethyl ether and n-hexane.

後処理

  1. temperatureSubsequently, the mixture is heated for 1.5 hours
  2. temperatureat reflux temperature
  3. distillationThe ethanol is distilled off in a water jet vacuum
  4. extractionthe residue is extracted repeatedly with ether
  5. washThe combined ethereal phases are washed repeatedly with water
  6. dry with materialdried over sodium sulfate
  7. distillationthe ther is distilled off entirely
  8. customThe crude oxime is chromatographed over silica gel (eluant
  9. additiona 1:1 mixture of diethyl ether and n-hexane)
  10. customThe resultant 4-(4-phenoxyphenyl)-2-butanone oxime melts at 80°-82° C. after recrystallisation
  11. additionin a mixture of diethyl ether and n-hexane

出典と根拠

ORDレコード
ord-6beda3f88e7345d997eba55f398c8c65
出典データセット
uspto-grants-1988_08
特許番号
US04766152

反応ノート

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