Water → 1-{4-[2-(3-Carboxypropionyloxy)ethylaminocarbonyl]butyl}-5-ethyl-5-phenyl-2,4,6(1H,3H,5H)-pyrimidinetrione

HRID 1975241노트

반응식

HRID 1975241 반응식
[CH2:1]([C:3]1([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:8](=[O:9])[N:7]([CH2:10][CH2:11][CH2:12][CH2:13][C:14]([NH:16][CH2:17][CH2:18][OH:19])=[O:15])[C:6](=[O:20])[NH:5][C:4]1=[O:21])[CH3:2].[C:28]1(=[O:34])[O:33][C:31](=[O:32])[CH2:30][CH2:29]1.CN(C1C=CC=CN=1)C.O>C(Cl)(Cl)Cl.ClCCl>[C:31]([CH2:30][CH2:29][C:28]([O:19][CH2:18][CH2:17][NH:16][C:14]([CH2:13][CH2:12][CH2:11][CH2:10][N:7]1[C:8](=[O:9])[C:3]([CH2:1][CH3:2])([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:4](=[O:21])[NH:5][C:6]1=[O:20])=[O:15])=[O:34])([OH:33])=[O:32]

참가 물질

7

반응물 4

HCID 962WaterHCID 7922Succinic anhydrideHCID 218852-DimethylaminopyridineHCID 199751925-Ethyl-1-[4-(2-hydroxyethylaminocarbonyl)butyl]-5-phenyl-2,4,6(1H,3H,5H)pyrimidinetrione

생성물 1

HCID 199751881-{4-[2-(3-Carboxypropionyloxy)ethylaminocarbonyl]butyl}-5-ethyl-5-phenyl-2,4,6(1H,3H,5H)-pyrimidinetrione

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매

실험 절차

A mixture of the product from step 1 (2.9 g, 0.007 mole), succinic anhydride (0.7 g, 0.007 mole), and dimethylaminopyridine (0.9 g, 0.007 mole) in chloroform (100 mL) was heated with hot water (50°-60° C.) for 30 min and then stirred at room temperature for 3 days. Dichloromethane (300 mL) was added, and the mixture was washed with 10% hydrochloric acid solution (2×100 mL), washed with saturated sodium chloride solution (100 mL), dried over anhydrous magnesium sulfate, filtered, and solvent removed to give an oil which was used directly in the next step.

후처리

  1. washthe mixture was washed with 10% hydrochloric acid solution (2×100 mL)
  2. washwashed with saturated sodium chloride solution (100 mL)
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customsolvent removed
  6. customto give an oil which

출처 및 근거

ORD 기록
ord-d8df72bbc4d042e8b49908c0d93588ad
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05284948

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