Water → 1-(3,3-Dimethoxy-propyl)-5-(2,4-dimethyl-oxazol-5-yl)-1H-pyrimidine-2,4-dione

HRID 12692노트

반응식

HRID 12692 반응식
[CH3:1][C:2]1[O:3][C:4]([C:8]2[C:9](=[O:15])[NH:10][C:11](=[O:14])[NH:12][CH:13]=2)=[C:5]([CH3:7])[N:6]=1.C([O-])([O-])=O.[K+].[K+].Br[CH2:23][CH2:24][CH:25]([O:28][CH3:29])[O:26][CH3:27].O>CN(C=O)C>[CH3:27][O:26][CH:25]([O:28][CH3:29])[CH2:24][CH2:23][N:12]1[CH:13]=[C:8]([C:4]2[O:3][C:2]([CH3:1])=[N:6][C:5]=2[CH3:7])[C:9](=[O:15])[NH:10][C:11]1=[O:14]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 1189323-Bromopropionaldehyde dimethylacetalHCID 589942315-(2,4-Dimethyl-oxazol-5-yl)-1H-pyrimidine-2,4-dione

생성물 1

HCID 589941601-(3,3-Dimethoxy-propyl)-5-(2,4-dimethyl-oxazol-5-yl)-1H-pyrimidine-2,4-dione수율 53%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

5-(2,4-Dimethyl-oxazol-5-yl)-1H-pyrimidine-2,4-dione (Prep62, 480 mg, 2.32 mmol) and K2CO3 (320 mg, 2.32 mmol) were suspended in dry DMF (6 ml) and stirred at room temperature for 1 h. A solution of 3-bromo-1,1dimethoxy-propane (467 mg, 2.55 mmol) in dry DMF (2 mL) was added dropwise and the mixture stirred at room temperature for 72 hours. Water (80 mL) was added and the product extracted with ethyl acetate. The organic phase was dried (Na2SO4) and evaporated to give 377 mg of the final compound that was used without any other purification in the next step (53% yield).

후처리

  1. stirringthe mixture stirred at room temperature for 72 hours
  2. extractionthe product extracted with ethyl acetate
  3. dry with materialThe organic phase was dried (Na2SO4)
  4. customevaporated

출처 및 근거

ORD 기록
ord-4f6497a025c44772aa97628a9417757c
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07727988B2

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