Water → 1-(3,3-Dimethoxy-propyl)-5-(6-fluoro-pyridin-2-yl)-1H-pyrimidine-2,4-dione

HRID 12705노트

반응식

HRID 12705 반응식
Cl.[F:2][C:3]1[N:8]=[C:7]([C:9]2[C:10](=[O:16])[NH:11][C:12](=[O:15])[NH:13][CH:14]=2)[CH:6]=[CH:5][CH:4]=1.C([O-])([O-])=O.[K+].[K+].Br[CH2:24][CH2:25][CH:26]([O:29][CH3:30])[O:27][CH3:28].O>CN(C=O)C>[CH3:28][O:27][CH:26]([O:29][CH3:30])[CH2:25][CH2:24][N:13]1[CH:14]=[C:9]([C:7]2[CH:6]=[CH:5][CH:4]=[C:3]([F:2])[N:8]=2)[C:10](=[O:16])[NH:11][C:12]1=[O:15]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 1189323-Bromopropionaldehyde dimethylacetalHCID 686903145-(6-Fluoro-pyridin-2-yl)-1H-pyrimidine-2,4-dione hydrochloride

생성물 1

HCID 589942011-(3,3-Dimethoxy-propyl)-5-(6-fluoro-pyridin-2-yl)-1H-pyrimidine-2,4-dione수율 70.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 5-(6-Fluoro-pyridin-2-yl)-1H-pyrimidine-2,4-dione hydrochloride (Prep75, 200 mg, 0.82 mmol), and K2CO3 (169 mg, 1.23 mmol) in DMF (4 ml) was stirred 1 hour at room temperature. 3-Bromo-1,1dimethoxy-propane (165 mg, 0.90 mmol) was added and stirring was continued for 48 hours. Water (50 ml) was added and the product was extracted with ethyl acetate. The organic phase was dried (Na2SO4) and evaporated. The crude was triturated with iPr2O to give 179 mg of the final compound as a white solid (70% yield).

후처리

  1. stirringstirring
  2. waitwas continued for 48 hours
  3. extractionthe product was extracted with ethyl acetate
  4. dry with materialThe organic phase was dried (Na2SO4)
  5. customevaporated
  6. customThe crude was triturated with iPr2O

출처 및 근거

ORD 기록
ord-e9f8b59231f648d7990315cef63ab5fc
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07727988B2

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