Ethanol → HCID 44549262、化合物

HRID 1512978ノート

反応式

HRID 1512978 の反応式
S(=O)(=O)(O)[OH:2].[C:6]([C:8]1[CH:13]=[C:12]([CH3:14])[C:11]([N+:15]([O-:17])=[O:16])=[CH:10][N:9]=1)#N.[CH2:18]([OH:20])[CH3:19]>>[CH3:14][C:12]1[C:11]([N+:15]([O-:17])=[O:16])=[CH:10][N:9]=[C:8]([C:6]([O:20][CH2:18][CH3:19])=[O:2])[CH:13]=1

参加物

4

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 230001714-Methyl-5-nitropyridine-2-carbonitrile

生成物 1

HCID 44549262HCID 44549262、化合物

反応条件

温度
120 °C

実験手順

To concentrated sulfuric acid (45 mL) was added ethanol (100 mL) under ice-cooling, followed by adding 2-cyano-4-methyl-5-nitropyridine (3.54 g), and the reaction vessel was equipped with a reflux condenser, and the mixture was stirred at 120° C. for 2 hours. The reaction mixture was cooled to room temperature. The reaction mixture was poured into ice, and the resulting mixture was extracted with diethyl ether. The water layer was extracted with methylene chloride. The extracts were combined, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=3/1) to give the title compound (3.23 g).

後処理

  1. temperaturecooling
  2. customthe reaction vessel was equipped with a reflux condenser
  3. temperatureThe reaction mixture was cooled to room temperature
  4. additionThe reaction mixture was poured into ice
  5. extractionthe resulting mixture was extracted with diethyl ether
  6. extractionThe water layer was extracted with methylene chloride
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customThe solvent was removed under reduced pressure
  9. customthe residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=3/1)

出典と根拠

ORDレコード
ord-ef4817d0cefb4cefa1413944faa800a3
出典データセット
uspto-grants-2012_07
特許番号
US08217069B2

反応ノート

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