Dimethylformamide diethylacetal → Ethyl 3-(N,N-dimethylamino)-2-(1H-imidazol-1-yl)acrylate

HRID 562447ノート

反応式

HRID 562447 の反応式
[N:1]1([CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH:5]=[CH:4][N:3]=[CH:2]1.C(O[CH:15](OCC)[N:16]([CH3:18])[CH3:17])C>>[CH3:15][N:16]([CH:18]=[C:6]([N:1]1[CH:5]=[CH:4][N:3]=[CH:2]1)[C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH3:17]

参加物

3

反応物 2

HCID 70913Dimethylformamide diethylacetalHCID 3798501ethyl 2-(1H-imidazol-1-yl)acetate

生成物 1

HCID 66726242Ethyl 3-(N,N-dimethylamino)-2-(1H-imidazol-1-yl)acrylate

実験手順

38.0 g (244.9 mmol) of the compound from Example 3A are stirred in 126 ml (108.1 g, 734.7 mmol) of N,N-dimethylformamide diethyl acetal at a bath temperature of 90° C. for 16 h. After cooling, the mixture is concentrated under reduced pressure, the residue is stirred with diisopropyl ether and the solid is filtered off and finally washed with diisopropyl ether. Yield: 49.0 g (95% of theory)

後処理

  1. temperatureAfter cooling
  2. concentrationthe mixture is concentrated under reduced pressure
  3. filtrationthe solid is filtered off
  4. washfinally washed with diisopropyl ether

出典と根拠

ORDレコード
ord-f25bccf5087346a5946a6563ea7435c9
出典データセット
uspto-grants-2011_11
特許番号
US08067407B2

反応ノート

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