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

HRID 2426105노트

반응식

HRID 2426105 반응식
[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

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 178434472HCID 178434472, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-1534ab724aa8403085dbf0bcbf542ab2
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07968554B2

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