Dimethylformamide → HCID 178510459, 화합물

HRID 655680노트

반응식

HRID 655680 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 178510459HCID 178510459, 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% 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.

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-1dbeaa7924a040a0b77767dfffb33de8
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08071601B2

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