Hydroxyamine hydrochloride → HCID 136393701、化合物

HRID 1253282ノート

反応式

HRID 1253282 の反応式
C([O-])(=O)C.[Na+].Cl.[NH2:7][OH:8].[CH2:9]([O:11][C:12](=[O:26])[C:13](=O)[C:14]1[C:22]2[C:17](=[C:18]([CH2:23][CH3:24])[CH:19]=[CH:20][CH:21]=2)[NH:16][CH:15]=1)[CH3:10]>O.C(O)C>[CH2:9]([O:11][C:12](=[O:26])[C:13](=[N:7][OH:8])[C:14]1[C:22]2[C:17](=[C:18]([CH2:23][CH3:24])[CH:19]=[CH:20][CH:21]=2)[NH:16][CH:15]=1)[CH3:10]

参加物

6

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 14010219ethyl 2-(7-ethyl-1H-indol-3-yl)-2-oxoacetate

生成物 1

HCID 136393701HCID 136393701、化合物収率 75.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

Solutions of sodium acetate (43.7 g, 0.53 mol) in water (100 mL) and hydroxylamine hydrochloride (37 g, 0.53 mol) in water (100 mL) were added to 7-ethyl-α-oxo-1H-indole-3-acetic acid ethyl ester 4 (17.4 g, 0.07 mol), in ethanol (250 mL) and the mixture was heated at reflux for 12 hours. The ethanol was removed by distillation and the resultant precipitate was filtered and recrystallized from hot ethanol to give the product (13.8 g, 75%), m.p. 167°-169° C. as a mixture of isomers.

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 12 hours
  3. customThe ethanol was removed by distillation
  4. filtrationthe resultant precipitate was filtered
  5. customrecrystallized from hot ethanol

出典と根拠

ORDレコード
ord-282044119787497b8bf5285af2727d59
出典データセット
uspto-grants-1988_05
特許番号
US04748252

反応ノート

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