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

HRID 12701
ノート
印刷プレビュー

反応式

HRID 12701 の反応式
Cl.[Cl:2][C:3]1[C:8]([C:9]2[C:10](=[O:16])[NH:11][C:12](=[O:15])[NH:13][CH:14]=2)=[CH:7][C:6]([F:17])=[CH:5][N:4]=1.C([O-])([O-])=O.[K+].[K+].Br[CH2:25][CH2:26][CH:27]([O:30][CH3:31])[O:28][CH3:29].O>CN(C=O)C>[CH3:29][O:28][CH:27]([O:30][CH3:31])[CH2:26][CH2:25][N:13]1[CH:14]=[C:9]([C:8]2[C:3]([Cl:2])=[N:4][CH:5]=[C:6]([F:17])[CH:7]=2)[C:10](=[O:16])[NH:11][C:12]1=[O:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 1189323-Bromopropionaldehyde dimethylacetalHCID 866159455-(2-Chloro-5-fluoro-pyridin-3-yl)-1H-pyrimidine-2,4-dione hydrochloride

生成物 1

HCID 589941491-(3,3-Dimethoxy-propyl)-5-(2-chloro-5-fluoro-pyridin-3-yl)-1H-pyrimidine-2,4-dione収率 48.5%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

5-(2-Chloro-5-fluoro-pyridin-3-yl)-1H-pyrimidine-2,4-dione hydrochloride (Prep71, 249 mg, 0.9 mmol), K2CO3 (124 mg, 0.9 mmol) and 3-bromo-1,1dimethoxy-propane (205 mg, 1.1 mmol) were suspended in DMF (3 ml). After stirring the reaction at room temperature for 18 hours, water was added. The aqueous layer washed with diethylether and then the product was extracted with ethyl acetate. The organic phase was dried (Na2SO4) and evaporated to give 150 mg of the final compound that was used without further purification in the next step (48% yield).

後処理

  1. customthe reaction at room temperature for 18 hours
  2. washThe aqueous layer washed with diethylether
  3. extractionthe product was extracted with ethyl acetate
  4. dry with materialThe organic phase was dried (Na2SO4)
  5. customevaporated

出典と根拠

ORDレコード
ord-224de5a4eea7482e98c9b75bfc6eabe9
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07727988B2

反応ノート

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