Methanol → Methyl 6-aminonicotinate

HRID 130342

反応式

HRID 130342 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][N:3]=1.S(=O)(=O)(O)O.[CH3:16]O>>[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH3:16])=[O:7])=[CH:4][N:3]=1

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 184966-Aminonicotinic acid

生成物 1

HCID 737487Methyl 6-aminonicotinate収率 30%

実験手順

A suspension of 6-aminonicotinic acid (2.0 g, 14.5 mmol) and sulfuric acid (2 mL) in methanol (125 mL) was heated at reflux overnight. The solution was cooled, the methanol evaporated and the residue was taken up in water (100 mL) and made basic with NaHCO3 (s), causing a white solid to precipitate. The mixture was extracted with chloroform (3×40 mL) and the combined extracts were dried (MgSO4) and evaporated to afford the ester as an off-white solid (1.04 g, 30%).

後処理

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. temperatureThe solution was cooled
  4. customthe methanol evaporated
  5. customto precipitate
  6. extractionThe mixture was extracted with chloroform (3×40 mL)
  7. dry with materialthe combined extracts were dried (MgSO4)
  8. customevaporated

出典と根拠

ORDレコード
ord-9f98e989563b4806b1ae9fe134ab2502
出典データセット
uspto-grants-2008_06
特許番号
US07381734B2

関連ノート

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