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Dimethylformamide → HCID 178429869, 화합물

HRID 2195688
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HRID 2195688 반응식
C(#N)C([CH2:4][C:5]#[N:6])O.[H-].[Na+].[CH3:10][CH:11]1[O:16][CH:15]([CH3:17])[CH2:14][N:13]([C:18]2[CH:29]=[C:22]3[C:23]([O:25][C:26](=O)[NH:27][C:21]3=[CH:20][CH:19]=2)=O)[CH2:12]1.C[N:31](C)C=O>O>[NH2:31][C:26]1[C:4]([C:5]#[N:6])=[C:23]([OH:25])[C:22]2[C:21](=[CH:20][CH:19]=[C:18]([N:13]3[CH2:14][CH:15]([CH3:17])[O:16][CH:11]([CH3:10])[CH2:12]3)[CH:29]=2)[N:27]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 212535622-HydroxybutanedinitrileHCID 866445925-(2,6-Dimethylmorpholin-4-yl)isatoic anhydride

생성물 1

HCID 178429869HCID 178429869, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

4 g of malonitrile is dissolved in 50 ml of dimethylformamide. To the solution, in several portions, 2.4 g of 60% sodium hydride in oily dispersion are added. To the clear solution 8 g of 5-(2,6-dimethylmorpholin-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, and the pH is set to 6. The precipitated material is filtered off, washed with water. After drying 6.5 g of the title compound is obtained. (MH+: 299)

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-1406628a7fcb43afb1d23d682abba600
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08338411B2

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