Dimethylformamide → HCID 178473878、化合物

HRID 2195694ノート

反応式

HRID 2195694 の反応式
C(#N)C([CH2:4][C:5]#[N:6])O.[H-].[Na+].[C:10]([N:13]1[CH2:18][CH2:17][N:16]([C:19]2[CH:30]=[C:23]3[C:24]([O:26][C:27](=O)[NH:28][C:22]3=[CH:21][CH:20]=2)=O)[CH2:15][CH2:14]1)(=[O:12])[CH3:11].C[N:32](C)C=O>O>[NH2:32][C:27]1[C:4]([C:5]#[N:6])=[C:24]([OH:26])[C:23]2[C:22](=[CH:21][CH:20]=[C:19]([N:16]3[CH2:15][CH2:14][N:13]([C:10](=[O:12])[CH3:11])[CH2:18][CH2:17]3)[CH:30]=2)[N:28]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 212535622-HydroxybutanedinitrileHCID 866445955-(4-Acetylpiperazin-1-yl)isatoic anhydride

生成物 1

HCID 178473878HCID 178473878、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

4 g malonitrile is dissolved in 50 ml dimethylformamide and in several portions 2.4 g sodium hydride 60% dispersion is added to it. To the clear solution 8 g 5-(4-acetylpiperazin-1-yl)isatoic anhydride is added and the mixture is stirred at room temperature for 10 hours. The reaction mixture is diluted with 70 ml water and extracted with 2×30 ml ethyl acetate. The aqueous phase is evaporated to dryness at reduced pressure, the solid residue is dissolved in 20 ml water and the pH is adjusted to 6 with acetic acid. The precipitated material is filtered off and washed with water. After drying 6.5 g of the title compound is obtained (MH+: 312).

後処理

  1. additionis added to it
  2. extractionextracted with 2×30 ml ethyl acetate
  3. customThe aqueous phase is evaporated to dryness at reduced pressure
  4. dissolutionthe solid residue is dissolved in 20 ml water
  5. filtrationThe precipitated material is filtered off
  6. washwashed with water
  7. dry with materialAfter drying 6.5 g of the title compound
  8. customis obtained (MH+: 312)

出典と根拠

ORDレコード
ord-149eb52dbc834748862e406c6904ed90
出典データセット
uspto-grants-2012_12
特許番号
US08338411B2

反応ノート

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