Dimethylformamide → HCID 11230310, 화합물

HRID 1397632노트

반응식

HRID 1397632 반응식
[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]

참가 물질

5

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 15363167HCID 15363167, 화합물

생성물 1

HCID 11230310HCID 11230310, 화합물

실험 절차

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%).

후처리

  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%)

출처 및 근거

ORD 기록
ord-122e732abd3045709a63cf3df12fc2f6
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08901136B2

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