Trimethylsilyldiazomethane → Methyl 2-acetamidoisonicotinate

HRID 1740946

反応式

HRID 1740946 の反応式
[C:1]([C:4]1[CH:9]=[CH:8][N:7]=[C:6]([NH:10][C:11](=[O:13])[CH3:12])[CH:5]=1)([OH:3])=[O:2].[Si](C=[N+]=[N-])(C)(C)[CH3:15]>CO.C1C=CC=CC=1>[CH3:15][O:2][C:1]([C:4]1[CH:9]=[CH:8][N:7]=[C:6]([NH:10][C:11](=[O:13])[CH3:12])[CH:5]=1)=[O:3]

参加物

4

反応物 2

HCID 167693TrimethylsilyldiazomethaneHCID 37744662-Acetamidopyridine-4-carboxylic acid

生成物 1

HCID 22185175Methyl 2-acetamidoisonicotinate

試薬・触媒・溶媒 1

HCID 21927730Benzene methanol溶媒

実験手順

4-Carboxy-2-acetylaminopyridine (3.4 g, 19 mmol) was dissolved in methanol/benzene (100 mL, 1:1). TMS-diazomethane was added (1M, Aldrich) with cooling until the yellow color just persisted, then the solvent was removed under reduced pressure. The product was purified by silica gel column chromatography (50/50 hexane/ethyl acetate) and 3.0 g of product was recovered.

後処理

  1. temperaturewith cooling until the yellow color
  2. customthe solvent was removed under reduced pressure
  3. customThe product was purified by silica gel column chromatography (50/50 hexane/ethyl acetate) and 3.0 g of product
  4. customwas recovered

出典と根拠

ORDレコード
ord-5841a4b889fc4ec4832020a9bd18915c
出典データセット
uspto-grants-1999_10
特許番号
US05972975

関連ノート

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