Potassium Carbonate → HCID 178498306、化合物

HRID 1251915ノート

反応式

HRID 1251915 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]([C:14]([O:16][CH3:17])=[O:15])=[CH:12][CH:11]=[CH:10][N+:9]=2[O-])=[CH:4][CH:3]=1.C(=O)([O-])[O-:20].[K+].[K+]>C(OC(=O)C)(=O)C.CO.O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]([C:14]([O:16][CH3:17])=[O:15])=[CH:12][CH:11]=[C:10]([OH:20])[N:9]=2)=[CH:4][CH:3]=1

参加物

6

反応物 2

HCID 11430Potassium CarbonateHCID 183245012-(4-Fluorophenyl)-3-(methoxycarbonyl)pyridine-1-oxide

生成物 1

HCID 178498306HCID 178498306、化合物収率 76.2%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 7918Acetic Anhydride溶媒

実験手順

A solution of 2-(4-fluorophenyl)-3-(methoxycarbonyl)pyridine-1-oxide (10.5 g.) in acetic anhydride (500 ml.) was stirred at reflux for 17 hr., cooled, evaporated to dryness and the residue partitioned between saturated sodium bicarbonate solution and ethyl acetate. The organic layer was separated, dried and evaporated to dryness. The gum obtained was dissolved in methanol (400 ml.), treated with a solution of potassium carbonate (11.7 g.) in water (100 ml) and stirred at ambient temperature for 2 hours. The methanol was evaporated off, the aqueous residue diluted with more water (200 ml.) and the mixture filtered to give methyl 2-(4-fluorophenyl)-6-hydroxypyridin-3-carboxylate (8.0 g.) as a brown solid.

後処理

  1. temperatureat reflux for 17 hr
  2. temperature, cooled
  3. customevaporated to dryness
  4. customthe residue partitioned between saturated sodium bicarbonate solution and ethyl acetate
  5. customThe organic layer was separated
  6. customdried
  7. customevaporated to dryness
  8. customThe gum obtained
  9. customThe methanol was evaporated off
  10. additionthe aqueous residue diluted with more water (200 ml.)
  11. filtrationthe mixture filtered

出典と根拠

ORDレコード
ord-c10c598bafa443a9814c801f8a285ca6
出典データセット
uspto-grants-2002_01
特許番号
US06342765B1

反応ノート

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