Dimethylformamide → HCID 11230310、化合物

HRID 1678025ノート

反応式

HRID 1678025 の反応式
[Cl:1][C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[NH:4][C:5]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[N:6]2.[CH3:17]N(C=O)C.[H-].[Na+].CI>>[Cl:1][C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[N:4]=[C:5]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[N:6]2[CH3:17]

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 15363167HCID 15363167、化合物

生成物 1

HCID 11230310HCID 11230310、化合物

実験手順

To a solution of 6-chloro-8-phenyl-7H-purine (0.200 g, 0.000867 mol) (Example 109, step a) in DMF (8.0 mL, 0.10 mol) was added sodium hydride (0.025 g, 0.0010 mol). The mixture was stirred for 20 minutes and to this was added methyl iodide (0.065 mL, 0.0010 mol) and the mixture was stirred for 2 hours. The reaction was quenched by addition of saturated aqueous NH4Cl, and the mixture was extracted with ethyl acetate, washed with water, brine, dried (Na2SO4), filtered and concentrated. The residue was purified by flash chromatography (3 to 10% acetone/toluene) to obtain 145 mg (68%).

後処理

  1. stirringthe mixture was stirred for 2 hours
  2. customThe reaction was quenched by addition of saturated aqueous NH4Cl
  3. extractionthe mixture was extracted with ethyl acetate
  4. washwashed with water, brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was purified by flash chromatography (3 to 10% acetone/toluene)
  9. customto obtain 145 mg (68%)

出典と根拠

ORDレコード
ord-1409a69491fe4d55ba2f8745b3162fdc
出典データセット
uspto-grants-2011_08
特許番号
US08008307B2

反応ノート

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