Trifluoroacetic acid → 5-(1-Methyl-1H-pyrazol-4-yl)-3-(quinolin-6-ylmethyl)-3H-[1,2,3]triazolo[4,5-b]pyridin-7-amine
反応式
[NH2:1][C:2]1[C:3]([NH:22][CH2:23][C:24]2[CH:25]=[C:26]3[C:31](=[CH:32][CH:33]=2)[N:30]=[CH:29][CH:28]=[CH:27]3)=[N:4][C:5]([C:16]2[CH:17]=[N:18][N:19]([CH3:21])[CH:20]=2)=[CH:6][C:7]=1[NH:8]C(=O)OC(C)(C)C.[N:34]([O-])=O.[Na+].[OH-].[Na+].C(O)(C(F)(F)F)=O.C([O-])([O-])=O.[Na+].[Na+]>O.C(O)(=O)C>[CH3:21][N:19]1[CH:20]=[C:16]([C:5]2[N:4]=[C:3]3[N:22]([CH2:23][C:24]4[CH:25]=[C:26]5[C:31](=[CH:32][CH:33]=4)[N:30]=[CH:29][CH:28]=[CH:27]5)[N:34]=[N:1][C:2]3=[C:7]([NH2:8])[CH:6]=2)[CH:17]=[N:18]1参加物
8
反応物 5
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 0 °C
実験手順
tert-Butyl 3-amino-6-(1-methyl-1H-pyrazol-4-yl)-2-(quinolin-6-ylmethylamino)pyridin-4-ylcarbamate (890 mg, 2 mmol) was added to a solution of acetic acid (5 mL) and water (5 mL) at 0° C., followed by the addition of NaNO2 (300 mg, 4 mmol) in H2O (0.5 mL). The reaction was stirred at 0° C. for 1 h, then basified with 30% NaOH to pH=8. The resulting mixture was filtered to afford a solid. The solid was treated with TFA (3 mL), and then stirred at room temperature for another 0.5 h, before treated with aqueous Na2CO3 to adjust the pH to 8. The resulting mixture was purified by chromatography to afford the title compound (190 mg). MS: 358 (M+1)+.
後処理
- filtrationThe resulting mixture was filtered
- customto afford a solid
- stirringstirred at room temperature for another 0.5 h
- customThe resulting mixture was purified by chromatography
出典と根拠
- ORDレコード
- ord-ded026ece4224ad5a44d812cac1b9bfa
- 出典データセット
- uspto-grants-2013_08
- 特許番号
- US08507487B2
反応ノート
読み込み中…