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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Sodium Hydroxide → HCID 178425875, 화합물

HRID 968803
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HRID 968803 반응식
[CH:1]([NH:3][C:4]1[C:5]([N+:15]([O-])=O)=[C:6]([C:10](Br)=[CH:11][C:12]=1[CH3:13])[C:7]([OH:9])=[O:8])=O.[OH-].[Na+]>[Pd]>[CH3:13][C:12]1[C:4]2[NH:3][CH:1]=[N:15][C:5]=2[C:6]([C:7]([OH:9])=[O:8])=[CH:10][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 590163123-(Formylamino)-6-bromo-4-methyl-2-nitrobenzoic Acid

생성물 1

HCID 178425875HCID 178425875, 화합물

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

A mixture of 3-(Formylamino)-6-bromo-4-methyl-2-nitrobenzoic Acid (21) (1.055 g, 3.68 mmol) and palladium on carbon (10% Pd/C, 0.228 g) in aqueous NaOH (0.294 g, 7.35 mmol of solid NaOH in 100 mL of H2O) is hydrogenated under hydrogen pressure (40 psi) for about 16 hours. The reaction mixture is cooled to ambient temperature and filtered through a pad of Celite. The filtrate is acidified with HCO2H (about 25 mL) and heated to reflux for about 2 hours. The reaction mixture is cooled and concentrated in vacuo to give a beige solid. The solids are triturated in hot methanol (50 mL), cooled slowly to ambient temperature, and filtered to give 7-Methyl-1H-benzimidazole-4-carboxylic Acid (22), as beige solid (0.495 g, 81% yield).

후처리

  1. customfor about 16 hours
  2. filtrationfiltered through a pad of Celite
  3. temperatureheated
  4. temperatureto reflux for about 2 hours
  5. temperatureThe reaction mixture is cooled
  6. concentrationconcentrated in vacuo
  7. customto give a beige solid
  8. customThe solids are triturated in hot methanol (50 mL)
  9. temperaturecooled slowly to ambient temperature
  10. filtrationfiltered

출처 및 근거

ORD 기록
ord-42628da98f7b47ff8d6f21575b07c01d
출처 데이터셋
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07304084B2

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