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Hydroxyamine hydrochloride → HCID 76664802, 화합물

HRID 474897
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HRID 474897 반응식
Cl.[NH2:2][OH:3].C([O-])(=O)C.[Na+].[Br:9][C:10]1[CH:22]=[C:21]2[C:13]([C:14]3[CH2:15][CH2:16][CH2:17][C:18](=O)[C:19]=3[N:20]2[CH3:23])=[CH:12][CH:11]=1>CCO.O>[Br:9][C:10]1[CH:22]=[C:21]2[C:13]([C:14]3[CH2:15][CH2:16][CH2:17][C:18](=[N:2][OH:3])[C:19]=3[N:20]2[CH3:23])=[CH:12][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 58093399HCID 58093399, 화합물

생성물 1

HCID 76664802HCID 76664802, 화합물수율 90%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

Hydroxylamine hydrochloride (0.56 g, 8.1 mmol) and sodium acetate (0.66 g, 8.1 mmol) were added to a suspension of 7-bromo-9-methyl-2,3,4,9-tetrahydro-1H-carbazol-1-one (1.5 g, 5.4 mmol) in EtOH (14 mL) and H2O (5.0 mL), and the resulting suspension was heated at reflux for 18 h. The reaction was cooled and concentrated to dryness. The resulting solid was triturated with MeOH (100 mL), and the solids were dried to yield the title compound (1.4 g, 90%) as an off-white powder: 1H NMR (300 MHz, DMSO-d6) δ 11.14 (s, 1H), 7.66 (s, 1H), 7.47 (d, J=8.5 Hz, 1H), 7.15 (dd, J=8.5, 1.0 Hz, 1H), 3.95 (s, 3H), 2.79-2.72 (m, 4H), 1.88-1.83 (m, 2H).

후처리

  1. temperaturethe resulting suspension was heated
  2. temperatureat reflux for 18 h
  3. temperatureThe reaction was cooled
  4. concentrationconcentrated to dryness
  5. customThe resulting solid was triturated with MeOH (100 mL)
  6. customthe solids were dried

출처 및 근거

ORD 기록
ord-43fc116e85b642fc8887d66522e782de
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08637501B2

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