Dichloromethane → HCID 59173317、化合物
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
- concentrationconcentrated in vacuo
- dissolutionThe residue is dissolved in EtOAc
- washwashed with aqueous NaHCO3
- customThe organic layer is separated
- dry with materialdried with MgSO4
- 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
読み込み中…