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Sodium Hydroxide → HCID 178484274, 화합물

HRID 1886048
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HRID 1886048 반응식
[CH3:1][N:2]([CH2:11][CH2:12][N:13]([CH3:26])[C:14]1[NH:18][C:17]2[CH:19]=[CH:20][C:21]([N+:23]([O-])=O)=[CH:22][C:16]=2[N:15]=1)[C:3](=[O:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.O.O.Cl[Sn]Cl.[OH-].[Na+]>CCO>[CH3:1][N:2]([CH2:11][CH2:12][N:13]([CH3:26])[C:14]1[NH:18][C:17]2[CH:19]=[CH:20][C:21]([NH2:23])=[CH:22][C:16]=2[N:15]=1)[C:3](=[O:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 61436Stannous chloride dihydrateHCID 178484275HCID 178484275, 화합물

생성물 1

HCID 178484274HCID 178484274, 화합물수율 94.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of N-methyl-N-[2-[methyl(5-nitro-1H-benzimidazol-2-yl)amino]ethyl]benzamide (1.30 g, 3.68 mmol) and SnCl2.2H2O (4.15 g, 18.39 mmol) in EtOH (15 mL) was heated under reflux for 1 hour. The mixture was cooled and made basic (pH8) with 2.5N NaOH. The precipitate was removed by filtration and the filtrate was concentrated. The residue was stirred with EtOAc (150 mL) overnight, dried (MgSO4), and concentrated to give 1.12 g (94%) of a green foam.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 1 hour
  3. temperatureThe mixture was cooled
  4. customThe precipitate was removed by filtration
  5. concentrationthe filtrate was concentrated
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b170a3f7e7954ead93f3de87c93d82f3
출처 데이터셋
uspto-grants-1992_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05149700

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