Dimethylformamide → HCID 178482613、化合物

HRID 1715810ノート

反応式

HRID 1715810 の反応式
C(#N)C([CH2:4][C:5]#[N:6])O.[H-].[Na+].[CH3:10][N:11]([CH3:24])[C:12]1[CH:23]=[C:16]2[C:17]([O:19][C:20](=O)[NH:21][C:15]2=[CH:14][CH:13]=1)=O.C[N:26](C)C=O>O>[NH2:26][C:20]1[C:4]([C:5]#[N:6])=[C:17]([OH:19])[C:16]2[C:15](=[CH:14][CH:13]=[C:12]([N:11]([CH3:10])[CH3:24])[CH:23]=2)[N:21]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 127157955-Dimethylaminoisatoic anhydrideHCID 212535622-Hydroxybutanedinitrile

生成物 1

HCID 178482613HCID 178482613、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To the solution of 4 g of malonitrile in 50 mL of dimethylformamide in several portions 2.4 g of sodium hydride 60% oily dispersion is added. To the clear solution 8 g of 5-dimethylamino-isatoic anhydride is added and the mixture is stirred at room temperature for 10 hours. The mixture is diluted with 70 mL of water and extracted with 2×30 mL of ethyl acetate. The aqueous phase is evaporated in vacuum, the solid residue is dissolved in 20 mL of water, 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, m.p.: 360° C.

後処理

  1. extractionextracted with 2×30 mL of ethyl acetate
  2. customThe aqueous phase is evaporated in vacuum
  3. dissolutionthe solid residue is dissolved in 20 mL of water
  4. filtrationThe precipitated material is filtered off
  5. washwashed with water
  6. dry with materialAfter drying 6.5 g of the title compound
  7. customis obtained

出典と根拠

ORDレコード
ord-ffda11f3a09e4facaded07fb5f461211
出典データセット
uspto-grants-2010_09
特許番号
US07799922B2

反応ノート

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