Sulfuric Acid → HCID 178498115、化合物

HRID 416571ノート

反応式

HRID 416571 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.[C:16]1(C)C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+]>CO>[CH3:16][O:5][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][CH:9]=[N:10][C:2]=1[OH:1]

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 1140TolueneHCID 11430Potassium CarbonateHCID 178418543HCID 178418543、化合物

生成物 1

HCID 178498115HCID 178498115、化合物収率 84%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 2-hydroxynicotinic acid (3-067-01) (50 g) in methanol (500 ml) were added conc. sulfuric acid (15 ml) and toluene (100 mL) at room temperature. After the reaction mixture was stirred for 28 h attached Dienstark reflux tube and neutralized with an aqueous potassium carbonate solution, the solvent was evaporated. To the residue were added aqueous saturated ammonium chloride solution and chloroform, and the organic layer was separated, and the aqueous layer was extracted with chloroform. The combined organic layers were dried over anhydrous magnesium sulfate, and evaporated under reduced pressure to give 2-hydroxynicotinic acid methyl ester (3-067-02) (46 g, 84%) as a white solid.

後処理

  1. temperaturereflux tube
  2. customthe solvent was evaporated
  3. additionTo the residue were added aqueous saturated ammonium chloride solution and chloroform
  4. customthe organic layer was separated
  5. extractionthe aqueous layer was extracted with chloroform
  6. dry with materialThe combined organic layers were dried over anhydrous magnesium sulfate
  7. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-dc4e39f386264f54b331d1bb4335e178
出典データセット
uspto-grants-2012_01
特許番号
US08088924B2

反応ノート

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