Methanol → Methyl pyrimidine-5-carboxylate

HRID 1653700노트

반응식

HRID 1653700 반응식
[N:1]1[CH:6]=[C:5]([C:7]([OH:9])=[O:8])[CH:4]=[N:3][CH:2]=1.[CH3:10]O>>[CH3:10][O:8][C:7]([C:5]1[CH:6]=[N:1][CH:2]=[N:3][CH:4]=1)=[O:9]

참가 물질

3

반응물 2

HCID 887MethanolHCID 78346Pyrimidine-5-carboxylic acid

생성물 1

HCID 253902Methyl pyrimidine-5-carboxylate수율 77%

실험 절차

Crude pyrimidine-5-carboxylic acid (2.4 g, 19.38 mmol) was suspended in 100 ml methanol in a round bottom flask fitted with a reflux condenser, drying tube, and a dropping funnel, and 2.8 ml thionyl chloride was added dropwise with stirring. The suspension was stirred and refluxed overnight; then cooled to room temperature and the solvents evaporated in vacuo. Ice cold water (50 ml) was added, basified to pH 8 (sat. NaHCO3), and extracted with chloroform (3×50 ml). The organics were dried (MgSO4), filtered and evaporated in vacuo to yield 2.07 g crude yellow crystals (77%).

후처리

  1. customfitted with a reflux condenser
  2. customdrying tube, and a dropping funnel
  3. addition2.8 ml thionyl chloride was added dropwise
  4. stirringThe suspension was stirred
  5. temperaturerefluxed overnight
  6. customthe solvents evaporated in vacuo
  7. additionIce cold water (50 ml) was added
  8. extractionextracted with chloroform (3×50 ml)
  9. dry with materialThe organics were dried (MgSO4)
  10. filtrationfiltered
  11. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-8dbcd190e65849a4877afb38a40f49ff
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05403845

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