Hydrogen Peroxide → 5-Hydroxy-2-nitrobenzoic acid

HRID 631274

반응식

HRID 631274 반응식
[OH:1][C:2]1[CH:3]=[CH:4][C:5]([N+:10]([O-:12])=[O:11])=[C:6]([CH:9]=1)[CH:7]=[O:8].OO.[OH:15]S(O)(=O)=O>[OH-].[Na+]>[OH:1][C:2]1[CH:3]=[CH:4][C:5]([N+:10]([O-:12])=[O:11])=[C:6]([CH:9]=1)[C:7]([OH:15])=[O:8]

참가 물질

5

반응물 3

HCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 392115-Hydroxy-2-nitrobenzaldehyde

생성물 1

HCID 118825-Hydroxy-2-nitrobenzoic acid수율 94%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

To 5-hydroxy-2-nitrobenzaldehyde (1.0 g, 6.0 mmol) in 2.5M NaOH(aq) (10 mL) at 100° C. was added 35% H2O2 (12 mL) dropwise over 10 minutes and the mixture heated at reflux overnight. The solution was acidified with 10% H2SO4, extracted with EtOAc (2×100 mL), and the combined organic layers washed with H2O and brine, dried over MgSO4, filtered and concentrated in vacuo to give 5-hydroxy-2-nitrobenzoic acid (1.03 g, 5.63 mmol, 94%). LC-MS (ESI) m/z 182 (M−H)+.

후처리

  1. temperaturethe mixture heated
  2. temperatureat reflux overnight
  3. extractionextracted with EtOAc (2×100 mL)
  4. washthe combined organic layers washed with H2O and brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-878015e2b6214942a25247816193e54a
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09320739B2

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