Dimethylformamide → HCID 11230310、化合物

HRID 1747690ノート

反応式

HRID 1747690 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-e8b49b18637e4321b6e551899d37e3bd
出典データセット
uspto-grants-2015_10
特許番号
US09150525B2

反応ノート

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