2-Chloro-N-(5-methyl-1H-pyrazol-3-yl)pyrimidin-4-amine → HCID 178428253、化合物

HRID 475290ノート

反応式

HRID 475290 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:13]=[C:12]([CH3:14])[NH:11][N:10]=2)[CH:5]=[CH:4][N:3]=1.Cl.O1CCCCC1[N:22]1[C:26]2[CH:27]=[CH:28][C:29]([C@@H:31]([NH2:33])[CH3:32])=[CH:30][C:25]=2[N:24]=[CH:23]1>CCCCO>[NH:22]1[C:26]2[CH:27]=[CH:28][C:29]([C@@H:31]([NH:33][C:2]3[N:7]=[C:6]([NH:8][C:9]4[CH:13]=[C:12]([CH3:14])[NH:11][N:10]=4)[CH:5]=[CH:4][N:3]=3)[CH3:32])=[CH:30][C:25]=2[N:24]=[CH:23]1

参加物

4

反応物 2

HCID 231324822-Chloro-N-(5-methyl-1H-pyrazol-3-yl)pyrimidin-4-amineHCID 86694728HCID 86694728、化合物

生成物 1

HCID 178428253HCID 178428253、化合物

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

To a solution of 2-chloro-N-(5-methyl-1H-pyrazol-3-yl)pyrimidin-4-amine (105 mg, 0.5 mmol) in n-BuOH (2 mL) in a microwave vial was added 126 (184 mg, 0.75 mmol). To the solution was added dropwise TEA (0.21 mL, 1.5 mmol) and the vial sealed and irradiated in a in the microwave synthesizer at 110° C. for 6 h. The solvent was evaporated under reduced pressure and the crude residue was taken up in DCM (5 mL) and MeOH (5 mL) and the solvent was again concentrated in vacuo. The residue was diluted in DMF (1 mL) and filtered. The crude mixture was purified by reverse phase HPLC to afford 9 mg (5%) of I-121.

後処理

  1. customthe vial sealed
  2. customirradiated in a in the microwave synthesizer at 110° C. for 6 h
  3. customThe solvent was evaporated under reduced pressure
  4. concentrationMeOH (5 mL) and the solvent was again concentrated in vacuo
  5. additionThe residue was diluted in DMF (1 mL)
  6. filtrationfiltered
  7. customThe crude mixture was purified by reverse phase HPLC
  8. customto afford 9 mg (5%) of I-121

出典と根拠

ORDレコード
ord-9533f86c249340dfb14e0773ba11f379
出典データセット
uspto-grants-2014_01
特許番号
US08637537B2

反応ノート

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