Methanol → HCID 178498115、化合物

HRID 384100ノート

反応式

HRID 384100 の反応式
[OH:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH3:16]O>O>[OH:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([O:6][CH3:16])=[O:5]

参加物

5

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 178418543HCID 178418543、化合物

生成物 1

HCID 178498115HCID 178498115、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 2-hydroxynicotinic acid (3.0 g) in methanol 15 ml, 1 ml of concentrated sulfuric acid was added, and the reaction solution was heated to reflux for 2 hours. The reaction solution was cooled, then the solvent was distilled off under reduced pressure, and the residue obtained was diluted with water and extracted with chloroform. The combined organic layers were washed with a saturated aqueous sodium bicarbonate solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to afford the title compound as a pale pink solid.

後処理

  1. temperaturethe reaction solution was heated
  2. temperatureto reflux for 2 hours
  3. temperatureThe reaction solution was cooled
  4. distillationthe solvent was distilled off under reduced pressure
  5. customthe residue obtained
  6. extractionextracted with chloroform
  7. washThe combined organic layers were washed with a saturated aqueous sodium bicarbonate solution
  8. dry with materialdried over anhydrous sodium sulfate
  9. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-e58895fc25984385b6357a0fd5e599ec
出典データセット
uspto-grants-2013_02
特許番号
US08367708B2

反応ノート

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