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Methanol → HCID 67248245, 화합물

HRID 2208916
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HRID 2208916 반응식
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([C:10]=1[CH3:11])[C:7]([OH:9])=[O:8].OS(O)(=O)=O.[CH3:17]O>>[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([C:10]=1[CH3:11])[C:7]([O:9][CH3:17])=[O:8]
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참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 70606775-Amino-4-methylpyridine-3-carboxylic acid

생성물 1

HCID 67248245HCID 67248245, 화합물수율 75%

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온도
70 °C

실험 절차

To a stirred solution of 5-amino-4-methylnicotinic acid (5.0 g, 32 mmol) in methanol (75 mL), was added conc. H2SO4 (5 mL) slowly at room temperature. The mixture was stirred at 70° C. for 12 h. On completion, the solvent was removed under reduced pressure and the residue was neutralized with saturated NaHCO3 solution. Extraction was carried out using EtOAc; the combined organic layers were washed with water, brine and dried over anhydrous Na2SO4 and concentrated under reduced pressure to give the title compound (4.1 g, 75%) which used without further purification.

후처리

  1. customOn completion, the solvent was removed under reduced pressure
  2. extractionExtraction
  3. washthe combined organic layers were washed with water, brine
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-5f3f42014dcc4d8ca5894ca41a8cd248
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09376422B2

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