Methanol → Methyl 6-aminonicotinate

HRID 130342노트

반응식

HRID 130342 반응식
[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

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 184966-Aminonicotinic acid

생성물 1

HCID 737487Methyl 6-aminonicotinate수율 30%

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-9f98e989563b4806b1ae9fe134ab2502
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07381734B2

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