Nitric Acid → HCID 57742139, 화합물

HRID 660284노트

반응식

HRID 660284 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]([CH3:14])[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:5]=[CH:6][CH:7]=1.[N+:15]([O-])([OH:17])=[O:16].O>C(O)(=O)C>[OH:1][C:2]1[CH:3]=[C:4]([CH:8]([CH3:14])[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:5]=[CH:6][C:7]=1[N+:15]([O-:17])=[O:16]

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 962WaterHCID 13356241HCID 13356241, 화합물

생성물 1

HCID 57742139HCID 57742139, 화합물수율 30.8%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

A solution of Ethyl 2-(3-hydroxyphenyl)propanoate (2.51 g, 12.9 mmol) in acetic acid (20 mL) was added nitric acid (1.45 g, 13.8 mmol) in acetic acid (2 mL) at room temperature. Then the colorless oil changed to the dark brown oil after 1˜2 minutes stirred. The reaction mixture was stirred for 15 minutes at room temperature then poured into iced water (100 mL), and extracted with EtOAc. The organic layer was dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel using EtOAc:hexanes (1:6) as eluant. Yellow solid (m.p. 45-47° C.), yield: 30.8%

후처리

  1. waitThen the colorless oil changed to the dark brown oil after 1˜2 minutes
  2. stirringThe reaction mixture was stirred for 15 minutes at room temperature
  3. extractionextracted with EtOAc
  4. dry with materialThe organic layer was dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by flash column chromatography on silica gel

출처 및 근거

ORD 기록
ord-9b93fe913a9d40f08db30487e4ab5f3a
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084484B2

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