Nitric Acid → 2,4-Dihydroxy-5-nitrobenzoic acid

HRID 643930

반응식

HRID 643930 반응식
[N+:1]([O-:4])(O)=[O:2].[OH:5][C:6]1[CH:14]=[C:13]([OH:15])[CH:12]=[CH:11][C:7]=1[C:8]([OH:10])=[O:9]>CC(O)=O>[OH:5][C:6]1[CH:14]=[C:13]([OH:15])[C:12]([N+:1]([O-:4])=[O:2])=[CH:11][C:7]=1[C:8]([OH:10])=[O:9]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 14912,4-Dihydroxybenzoic Acid

생성물 1

HCID 166379152,4-Dihydroxy-5-nitrobenzoic acid

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
0 °C

실험 절차

To an ice cold stirred solution of nitric acid (70%, 28 mL) and AcOH (30 mL), is added portionwise 2,4-dihydroxybenzoic acid (7.7 g, 49.9 mmol). The mixture is stirred at 0° C. for 15 min and then slowly warmed to room temperature. The reaction becomes very exothermic and is cooled again in an ice bath to keep the mixture at approximately room temperature. The mixture is stirred at room temperature for 18 h. The resulting precipitate is filtered, washed with water, air dried, then washed with DCM and dried under reduced pressure to afford 2,4-dihydroxy-5-nitrobenzoic acid as a solid: (M−H)−=198.1.

후처리

  1. temperatureslowly warmed to room temperature
  2. temperatureis cooled again in an ice bath
  3. customat approximately room temperature
  4. stirringThe mixture is stirred at room temperature for 18 h
  5. filtrationThe resulting precipitate is filtered
  6. washwashed with water, air
  7. customdried
  8. washwashed with DCM
  9. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-9e199b0885ae48148977de179103fcb5
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07700633B2

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