Potassium Carbonate → 7-bromo-3-(2-methoxyethyl)pyrido[3,2-d]pyrimidin-4(3H)-one

HRID 1619373ノート

反応式

HRID 1619373 の反応式
[Br:1][C:2]1[CH:11]=[N:10][C:9]2[C:8](=[O:12])[NH:7][CH:6]=[N:5][C:4]=2[CH:3]=1.Br[CH2:14][CH2:15][O:16][CH3:17].C([O-])([O-])=O.[K+].[K+]>CC(C)=O.CN(C=O)C.O>[Br:1][C:2]1[CH:11]=[N:10][C:9]2[C:8](=[O:12])[N:7]([CH2:14][CH2:15][O:16][CH3:17])[CH:6]=[N:5][C:4]=2[CH:3]=1

参加物

7

反応物 3

HCID 11430Potassium CarbonateHCID 809722-Bromoethyl methyl etherHCID 1356820527-bromo-3H,4H-pyrido(3,2-d)pyrimidin-4-one

生成物 1

HCID 585743837-bromo-3-(2-methoxyethyl)pyrido[3,2-d]pyrimidin-4(3H)-one

試薬・触媒・溶媒 3

HCID 180Acetone溶媒HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A solution of 7-bromopyrido[3,2-d]pyrimidin-4(3H)-one (200 mg, 0.89 mmol), 1-bromo-2-methoxyethane (148 mg, 1.06 mmol) and K2CO3 (184 mg, 1.3 mmol) in acetone (10 mL) and DMF (3 mL) was stirred at room temperature for 4 h. Then the mixture was diluted with H2O (50 mL) and extracted with ethyl acetate (3×50 mL), the combined organic layers were washed with brine, dried over Na2SO4. After filtration and concentration, the residue was purified by silica gel chromatography to give the desired product. MS (ESI): 284, 286 (MH+).

後処理

  1. extractionextracted with ethyl acetate (3×50 mL)
  2. washthe combined organic layers were washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationAfter filtration and concentration
  5. customthe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-5556129192144d94a976a8a41126fefc
出典データセット
uspto-grants-2014_07
特許番号
US08772301B2

反応ノート

読み込み中…