Ethanol → Ethyl 3-hydroxypicolinate

HRID 429201노트

반응식

HRID 429201 반응식
[OH:1][C:2]1[C:3]([C:8]([OH:10])=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=1.S(=O)(=O)(O)O.O.[CH2:17](O)[CH3:18]>C1C=CC=CC=1>[OH:1][C:2]1[C:3]([C:8]([O:10][CH2:17][CH3:18])=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 702EthanolHCID 962WaterHCID 1118Sulfuric AcidHCID 134013-Hydroxypicolinic Acid

생성물 1

HCID 15080989Ethyl 3-hydroxypicolinate

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

3-Hydroxypicolinic acid (12.5 g, 900 mmol) was suspended in a mixture of ethanol (300 ml) and benzene (100 ml). Sulfuric acid (5 ml) was added and the reaction mixture was heated at reflux with azeotropic removal of water via Dean Stark trap. After the reaction was complete, the organics were removed in vacuo. The residue was dissolved in water, basified with sodium carbonate and extracted with ethyl acetate. The ethyl acetate layer was dried over magnesium sulfate, concentrated in vacuo to give ethyl 3-hydroxypicolinate (15 g).

후처리

  1. temperaturethe reaction mixture was heated
  2. customthe organics were removed in vacuo
  3. dissolutionThe residue was dissolved in water
  4. extractionextracted with ethyl acetate
  5. dry with materialThe ethyl acetate layer was dried over magnesium sulfate
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-98e1482c50a647dbaccdbcf66a441673
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06316464B1

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