2-Methoxyethanol → 2-Methyl-4-(2-methoxyethoxy)-6-(4-fluorophenyl)-pyrido[3,2-d]pyrimidine

HRID 1517451ノート

反応式

HRID 1517451 の反応式
[H-].[Na+].[CH3:3][C:4]1[N:5]=[C:6](Cl)[C:7]2[N:13]=[C:12]([C:14]3[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=3)[CH:11]=[CH:10][C:8]=2[N:9]=1.[CH3:22][O:23][CH2:24][CH2:25][OH:26]>>[CH3:3][C:4]1[N:5]=[C:6]([O:26][CH2:25][CH2:24][O:23][CH3:22])[C:7]2[N:13]=[C:12]([C:14]3[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=3)[CH:11]=[CH:10][C:8]=2[N:9]=1

参加物

4

反応物 3

HCID 80192-MethoxyethanolHCID 24758Sodium hydrideHCID 576983684-Chloro-6-(4-fluorophenyl)-2-methylpyrido[3,2-d]pyrimidine

生成物 1

HCID 576983182-Methyl-4-(2-methoxyethoxy)-6-(4-fluorophenyl)-pyrido[3,2-d]pyrimidine収率 88%

実験手順

Sodium hydride (80 mg of a 60% dispersion in mineral oil, 2.0 mmol) was added to 2-methoxyethanol (10 ml). The mixture was stirred at room temperature for 10 minutes. Then, 2-methyl-4-chloro-6-(4-fluorophenyl)-pyrido[3,2-d]pyrimidine (110 mg, 0.4 mmol) was added to this solution. The resulting mixture was stirred at room temperature for another 40 minutes. After concentration under reduced pressure, the residue was purified by silica gel flash chromatography, the mobile phase being a mixture of ethanol and dichloromethane, in a volume ratio of 1:100, affording the pure title compound (110 mg, yield 88%) as a white solid which was characterised as follows: MS (m/z): 314 ([M+H]+, 100).

後処理

  1. stirringThe resulting mixture was stirred at room temperature for another 40 minutes
  2. concentrationAfter concentration under reduced pressure
  3. customthe residue was purified by silica gel flash chromatography
  4. additiona mixture of ethanol and dichloromethane

出典と根拠

ORDレコード
ord-6946c400dab54daeb1960fc577e7733b
出典データセット
uspto-grants-2012_07
特許番号
US08232278B2

反応ノート

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