Dichloromethane → HCID 59173317、化合物

HRID 220097ノート

反応式

HRID 220097 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8]C(=O)OC(C)(C)C)=[CH:4][C:3]=1[NH:16][C:17]1[N:21]([C:22]2[CH:27]=[C:26]([NH:28][CH3:29])[N:25]=[CH:24][N:23]=2)[N:20]=[C:19]([CH3:30])[CH:18]=1.C(Cl)Cl>C(O)(C(F)(F)F)=O>[CH3:1][C:2]1[C:3]([NH:16][C:17]2[N:21]([C:22]3[CH:27]=[C:26]([NH:28][CH3:29])[N:25]=[CH:24][N:23]=3)[N:20]=[C:19]([CH3:30])[CH:18]=2)=[CH:4][C:5]([NH2:8])=[CH:6][CH:7]=1

参加物

4

実験手順

Tert-butyl 4-methyl-3-(3-methyl-1-(6-(methylamino)pyrimidin-4-yl)-1H-pyrazol-5-ylamino)phenylcarbamate 38 (2.0 g) is dissolved in a mixed solvent of TFA:DCM/1:1 (20 mL). The mixture is stirred at room temperature for 4 hours, then concentrated in vacuo. The residue is dissolved in EtOAc and washed with aqueous NaHCO3. The organic layer is separated, dried with MgSO4, then concentrated in vacuo to provide 6-methyl-N1-(3-methyl-1-(6-(methylamino)pyrimidin-4-yl)-1H-pyrazol-5-yl)benzene-1,3-diamine 39.

後処理

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residue is dissolved in EtOAc
  3. washwashed with aqueous NaHCO3
  4. customThe organic layer is separated
  5. dry with materialdried with MgSO4
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c48fe1d8ab9a441eb8b304ffacea858a
出典データセット
uspto-grants-2012_06
特許番号
US08202876B2

反応ノート

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