Hydroxyamine hydrochloride → HCID 136393701, 화합물

HRID 1253282노트

반응식

HRID 1253282 반응식
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]

참가 물질

6

반응물 3

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

생성물 1

HCID 136393701HCID 136393701, 화합물수율 75.7%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-282044119787497b8bf5285af2727d59
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04748252

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