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Methanol → 2-(Methoxycarbonyl)pyridine-4-carboxylic acid

HRID 1838242
ノート
印刷プレビュー

反応式

HRID 1838242 の反応式
S(=O)(=O)(O)O.[N:6]1[CH:11]=[CH:10][C:9]([C:12]([OH:14])=[O:13])=[CH:8][C:7]=1[C:15]([OH:17])=[O:16].[CH3:18]O>>[CH3:18][O:16][C:15]([C:7]1[CH:8]=[C:9]([CH:10]=[CH:11][N:6]=1)[C:12]([OH:14])=[O:13])=[O:17]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 103652,4-Pyridinedicarboxylic acid

生成物 1

HCID 187533102-(Methoxycarbonyl)pyridine-4-carboxylic acid

反応条件

温度
5 °C

実験手順

A 1.7 ml portion of concentrated sulfuric acid was added to 50 ml of methanol solution containing 5.0 g of pyridine-2,4-dicarboxylic acid, and the mixture was heated under reflux for 1 hour and 10 minutes. After cooling, this was poured into ice water and stirred at 5° C. for 3 hours, and the thus precipitated white solid was collected by filtration. A 5.7 g portion of this product was dissolved in 100 ml of methanol with heating, and the solution was cooled and then stirred at room temperature. By collecting the thus precipitated white solid by filtration, 2.5 g of the title compound was obtained.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1 hour and 10 minutes
  3. temperatureAfter cooling
  4. filtrationthe thus precipitated white solid was collected by filtration
  5. dissolutionA 5.7 g portion of this product was dissolved in 100 ml of methanol
  6. temperaturewith heating
  7. temperaturethe solution was cooled
  8. stirringstirred at room temperature
  9. customBy collecting the thus precipitated white solid
  10. filtrationby filtration

出典と根拠

ORDレコード
ord-2faf7a35497c46e2877df3934cd2ac4a
出典データセット
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06673799B1

反応ノート

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