Methyl iodide → 4-chloro-1,3-dimethyl-1H-pyrazolo[3,4-d]pyrimidine

HRID 2426105ノート

反応式

HRID 2426105 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]2[NH:8][N:9]=[C:10]([CH3:11])[C:3]=12.[C:12](=O)([O-])[O-].[K+].[K+].IC>CN(C)C=O.C(OCC)(=O)C>[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]2[N:8]([CH3:12])[N:9]=[C:10]([CH3:11])[C:3]=12

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 178434472HCID 178434472、化合物

生成物 1

HCID 131255724-chloro-1,3-dimethyl-1H-pyrazolo[3,4-d]pyrimidine

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a mixture of 4-chloro-3-methyl-1H-pyrazolo[3,4-d]pyrimidine (150.4 mg, 0.89 mmol, Example 3) and potassium carbonate (187 mg, 1.35 mmol) in dimethylformamide (6 mL) was added iodomethane (225 mg, 1.59 mmol, Aldrich). The reaction mixture was stirred at room temperature for 2 hours before it was diluted with ethyl acetate, washed with water, brine, dried and concentrated. The crude product was purified by flash chromatography (silica gel, hexanes-ethyl acetate, 90/10 to 60/40) to give 4-chloro-1,3-dimethyl-1H-pyrazolo[3,4-d]pyrimidine as a white solid. (Yield 162.3 mg).

後処理

  1. washwashed with water, brine
  2. customdried
  3. concentrationconcentrated
  4. customThe crude product was purified by flash chromatography (silica gel, hexanes-ethyl acetate, 90/10 to 60/40)

出典と根拠

ORDレコード
ord-1534ab724aa8403085dbf0bcbf542ab2
出典データセット
uspto-grants-2011_06
特許番号
US07968554B2

反応ノート

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