Hydrochloric Acid → Methyl 3-benzyloxy-6-methoxypicolinate

HRID 350655노트

반응식

HRID 350655 반응식
[CH2:1]([O:8][C:9]1[C:10]([C:16]([O:18][CH3:19])=[O:17])=[N:11][C:12]([OH:15])=[CH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:20](=O)([O-])[O-].[K+].[K+].Cl>CC(C)=O.CI>[CH2:1]([O:8][C:9]1[C:10]([C:16]([O:18][CH3:19])=[O:17])=[N:11][C:12]([O:15][CH3:20])=[CH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 178499129HCID 178499129, 화합물

생성물 1

HCID 22175139Methyl 3-benzyloxy-6-methoxypicolinate수율 49%

시약·촉매·용매 2

HCID 180Acetone용매HCID 6328Methyl iodide용매

실험 절차

Methyl 3-benzyloxy-6-hydroxy-picolinate (0.55 g) was dissolved in 55 ml of acetone and 20 ml of methyl iodide. Potassium carbonate (1.4 g) was added to the solution, and the mixture was refluxed for 3 hr. After cooling, the reaction solution was neutralized with 1 N hydrochloric acid, and was concentrated under the reduced pressure. Methylene chloride and water were then added to the concentrate to conduct extraction. The organic layer was dried over magnesium sulfate, and the dried organic layer was then concentrated under the reduced pressure. The residue was purified by column chromatography (chloroform-methanol) to give 0.28 g (yield 49%) of the title compound.

후처리

  1. temperaturethe mixture was refluxed for 3 hr
  2. temperatureAfter cooling
  3. concentrationwas concentrated under the reduced pressure
  4. additionMethylene chloride and water were then added to the
  5. concentrationconcentrate
  6. extractionextraction
  7. dry with materialThe organic layer was dried over magnesium sulfate
  8. concentrationthe dried organic layer was then concentrated under the reduced pressure
  9. customThe residue was purified by column chromatography (chloroform-methanol)

출처 및 근거

ORD 기록
ord-0db6c987627c41fea65370e577ffed10
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07183278B1

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