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Ammonia → HCID 17848708, 화합물

HRID 457877
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HRID 457877 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:8]2[C:13]([C:14]3[CH:19]=[CH:18][N:17]=[C:16](F)[CH:15]=3)=[CH:12][N:11]=[C:10]([NH2:21])[N:9]=2)[CH:5]=[CH:6][CH:7]=1.[NH3:22].C(O)C.N>C(O)C>[NH2:22][C:16]1[CH:15]=[C:14]([C:13]2[C:8]([C:4]3[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[CH:3]=3)=[N:9][C:10]([NH2:21])=[N:11][CH:12]=2)[CH:19]=[CH:18][N:17]=1
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참가 물질

5

반응물 3

HCID 222AmmoniaHCID 17848732HCID 17848732, 화합물HCID 22020343Ethanol, reaction products with ammonia, distn. residues

생성물 1

HCID 17848708HCID 17848708, 화합물수율 12%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
150 °C

실험 절차

A mixture of 4-(3-fluorophenyl)-5-(2-fluoro-4-pyridyl)-2-pyrimidinylamine (100 mg, 0.352 mmol) and ammonia/ethanol (ethanol saturated with an ammonia gas under ice-cooling) (20 mL) was sealed in a test tube and stirred at 150° C. for 2 weeks. After cooling as it was, the reaction solution was concentrated. The residue was dissolved by adding ethyl acetate and water thereto. The organic layer was washed with water and brine, and then dried over anhydrous sodium sulfate and concentrated. The residue was purified by TLC plate (eluting solvent: dichloromethane/methanol=10/1), to give the title compound (12 mg, 12%).

후처리

  1. temperaturecooling) (20 mL)
  2. customwas sealed in a test tube
  3. temperatureAfter cooling as it
  4. concentrationthe reaction solution was concentrated
  5. dissolutionThe residue was dissolved
  6. additionby adding ethyl acetate and water
  7. washThe organic layer was washed with water and brine
  8. dry with materialdried over anhydrous sodium sulfate
  9. concentrationconcentrated
  10. customThe residue was purified by TLC plate (eluting solvent: dichloromethane/methanol=10/1)

출처 및 근거

ORD 기록
ord-e80391f8c20649d2983756ad1c0c2f0b
출처 데이터셋
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07189717B2

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