Methanol → HCID 46311240, 화합물

HRID 384117노트

반응식

HRID 384117 반응식
[Cl:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=[O:9])[C:5]([F:11])=[CH:4][CH:3]=1.[OH-].[Na+].[CH3:14]O>S(=O)(=O)(O)O>[CH3:14][O:9][C:8]([C:6]1[C:5]([F:11])=[CH:4][CH:3]=[C:2]([Cl:1])[N:7]=1)=[O:10]

참가 물질

5

반응물 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 447547876-Chloro-3-fluoropyridine-2-carboxylic acid

생성물 1

HCID 46311240HCID 46311240, 화합물

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

To a solution of 6-chloro-3-fluoropyridin-2-carboxylic acid (250 mg) in methanol (3 ml), 0.3 ml of concentrated sulfuric acid was added, and the reaction solution was heated to reflux for 2.5 hours. The reaction solution was cooled, and then the solvent was distilled off under reduced pressure. To the residue obtained was added 1N aqueous sodium hydroxide, and the mixture was extracted with ethyl acetate. The combined organic layers were washed with a saturated saline solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to afford the title compound as a white solid.

후처리

  1. temperaturethe reaction solution was heated
  2. temperatureto reflux for 2.5 hours
  3. temperatureThe reaction solution was cooled
  4. distillationthe solvent was distilled off under reduced pressure
  5. customTo the residue obtained
  6. extractionthe mixture was extracted with ethyl acetate
  7. washThe combined organic layers were washed with a saturated saline solution
  8. dry with materialdried over anhydrous sodium sulfate
  9. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-f3b65c4193f94445984acb887c6a9c9b
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367708B2

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