Dimethylformamide → HCID 178482613, 화합물

HRID 655695노트

반응식

HRID 655695 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 178482613HCID 178482613, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-353458c2d51d49e0a01fbd64d8206e7d
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08071601B2

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