2-Nitro-4-(thiophen-2-yl)aniline → 4-(Thiophen-2-yl)benzene-1,2-diamine
反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[CH:12]=[CH:11][C:9]([NH2:10])=[C:8]([N+:13]([O-])=O)[CH:7]=1.[H][H]>[Pd]>[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[CH:7]=[C:8]([NH2:13])[C:9]([NH2:10])=[CH:11][CH:12]=1参加物
4
実験手順
To a solution of 4-thienyl-2-nitroaniline (1 equiv, 400 mg, 1.82 mmol) was added 10% Pd/C (0.05 equiv, 97 mg, 0.09 mmol). The resulting suspension was stirred for overnight over 1 atm of hydrogen. The solids were filtered through celite pad and the filtrate was concentrated under vacuum. The crude material was purified by silica gel column chromatography with gradient of MeOH (0-10%) in CH2Cl2 to afford compound 30 (310 mg, 90%) and a white solid. LRMS (ESI): (calc) 190.2 (found) 191.0 (MH)+.
後処理
- filtrationThe solids were filtered through celite pad
- concentrationthe filtrate was concentrated under vacuum
- customThe crude material was purified by silica gel column chromatography with gradient of MeOH (0-10%) in CH2Cl2
出典と根拠
- ORDレコード
- ord-037a3ffdd9f646d0a19cd473696eb089
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09096565B2
反応ノート
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