Ethanol → Ethyl 2-methoxy-6-nitrophenylacetate

HRID 37869ノート

反応式

HRID 37869 の反応式
S(=O)(=O)(O)[OH:2].[CH3:6][O:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([N+:14]([O-:16])=[O:15])[C:9]=1[CH2:17][C:18]#N.[CH2:20]([OH:22])[CH3:21]>>[CH2:20]([O:22][C:18](=[O:2])[CH2:17][C:9]1[C:10]([N+:14]([O-:16])=[O:15])=[CH:11][CH:12]=[CH:13][C:8]=1[O:7][CH3:6])[CH3:21]

参加物

4

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 5550182-(2-Methoxy-6-nitrophenyl)acetonitrile

生成物 1

HCID 58216762Ethyl 2-methoxy-6-nitrophenylacetate収率 72%

実験手順

Sulfuric acid (1 mL) was slowly added to a solution of (2-methoxy-6-nitro-phenyl)-acetonitrile (200 mg, 1.04 mmol) in 95% ethanol (2 mL). The mixture was heated at reflux overnight then quenched into ice cold water and extracted with diethyl ether (10 mL). The organic phase was washed with water (2×10 mL), dried over anhydrous sodium sulfate and concentrated in vacuo to afford (2-methoxy-6-nitro-phenyl)-acetic acid ethyl ester (180 mg, 72%).

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux overnight
  3. customthen quenched into ice cold water
  4. extractionextracted with diethyl ether (10 mL)
  5. washThe organic phase was washed with water (2×10 mL)
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-202240da0fa5439b9bc95d88814baa97
出典データセット
uspto-grants-2013_09
特許番号
US08524705B2

反応ノート

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