Dimethylformamide → HCID 178510459、化合物

HRID 1985663ノート

反応式

HRID 1985663 の反応式
C(#N)C([CH2:4][C:5]#[N:6])O.[H-].[Na+].[N:10]1([C:16]2[CH:27]=[C:20]3[C:21]([O:23][C:24](=O)[NH:25][C:19]3=[CH:18][CH:17]=2)=O)[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1.C[N:29](C)C=O>O>[NH2:29][C:24]1[C:4]([C:5]#[N:6])=[C:21]([OH:23])[C:20]2[C:19](=[CH:18][CH:17]=[C:16]([N:10]3[CH2:11][CH2:12][O:13][CH2:14][CH2:15]3)[CH:27]=2)[N:25]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 212535622-HydroxybutanedinitrileHCID 866077765-(Morpholin-4-yl)isatoic anhydride

生成物 1

HCID 178510459HCID 178510459、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

4 g of malonitrile is dissolved in 50 mL of dimethylformamide. To the solution, in several portions, 2.4 g of 60% oily dispersion of sodium hydride are added. To the clear solution 8 g of 5-(morpholin-4-yl)isatoic anhydride is added and the mixture is stirred at room temperature for 10 hours. The reaction 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, washed with water. After drying 6.5 g of the title compound is obtained, m.p.: 291° 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-bb3a9b1d90b641158c79b2500c34699c
出典データセット
uspto-grants-2009_06
特許番号
US07547696B2

反応ノート

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