1-Butanol → 1-(4-(4-(4-(4-(Aminomethyl)piperidin-1-yl)-5-fluoropyrimidin-2-ylamino)phenyl)piperazin-1-yl)ethanone
反応式
Cl[C:2]1[N:7]=[C:6](Cl)[C:5]([F:9])=[CH:4][N:3]=1.C([N:12]([CH2:15][CH3:16])[CH2:13][CH3:14])C.[NH2:17][C:18]1[CH:23]=[CH:22][C:21]([N:24]2[CH2:29][CH2:28][N:27]([C:30](=[O:32])[CH3:31])[CH2:26][CH2:25]2)=[CH:20][CH:19]=1.C(O)CCC.[CH3:38][C:39]#[N:40]>>[NH2:40][CH2:39][CH:38]1[CH2:14][CH2:13][N:12]([C:6]2[C:5]([F:9])=[CH:4][N:3]=[C:2]([NH:17][C:18]3[CH:19]=[CH:20][C:21]([N:24]4[CH2:25][CH2:26][N:27]([C:30](=[O:32])[CH3:31])[CH2:28][CH2:29]4)=[CH:22][CH:23]=3)[N:7]=2)[CH2:15][CH2:16]1参加物
6
実験手順
A mixture of 2,4-dichloro-5-fluoropyrimidine (167 mg, 1.00 mmol), 4-N-Boc-aminomethyl piperidine (214 mg, 1.00 mmol) and triethylamine (0.300 mL, 2.15 mmol) in CH3CN (4 mL) was stirred at room temperature for 20 h. It was concentrated in vacuo. The residue was dissolved in nBuOH (6 mL). 2 mL of the nBuOH solution was taken, to which 1-(4-(4-aminophenyl)piperazin-1-yl)ethanone (108 mg, 0.49 mmol) was added. The solution was stirred at 116° C. for 20 h. nBuOH was removed in vacuo. The residue was dissolved in TFA (2 mL). After being stirred at room temperature for 2 h, TFA was removed in vacuo. The residue was purified by HPLC to give the titled compound (43 mg). MS 428.6 (M+H); UV 206.8, 265.8 nm.
後処理
- concentrationIt was concentrated in vacuo
- dissolutionThe residue was dissolved in nBuOH (6 mL)
- additionwas added
- customwas removed in vacuo
- dissolutionThe residue was dissolved in TFA (2 mL)
- stirringAfter being stirred at room temperature for 2 h
- customTFA was removed in vacuo
- customThe residue was purified by HPLC
出典と根拠
- ORDレコード
- ord-657bdb18136f47e28fdc88b5e1b3b521
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09139581B2
反応ノート
読み込み中…