Hydrochloric Acid → Methyl 3-benzyloxy-6-methoxypicolinate

HRID 350655ノート

反応式

HRID 350655 の反応式
[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

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 178499129HCID 178499129、化合物

生成物 1

HCID 22175139Methyl 3-benzyloxy-6-methoxypicolinate収率 49%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 6328Methyl iodide溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-0db6c987627c41fea65370e577ffed10
出典データセット
uspto-grants-2007_02
特許番号
US07183278B1

反応ノート

読み込み中…