5-Morpholino-2-nitroaniline → 4-(Morpholin-4-yl)benzene-1,2-diamine
反応式
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:8]=[CH:9][C:10]([N+:14]([O-])=O)=[C:11]([CH:13]=2)[NH2:12])[CH2:3][CH2:2]1.[H][H]>C(O)C.[Pd]>[O:1]1[CH2:2][CH2:3][N:4]([C:7]2[CH:13]=[C:11]([NH2:12])[C:10]([NH2:14])=[CH:9][CH:8]=2)[CH2:5][CH2:6]1参加物
5
実験手順
5-Morpholino-2-nitroaniline (200 mg, 0.896 mmol) was added to the 10% Pd/C (25 mg) in ethanol (25 mL) and then hydrogen gas (60 psi) was applied for overnight at room temperature. The reaction mixture was filtered through Celite, and the solvent was removed in vacuum. Purification by flash chromatography (5% CH3OH/CH2Cl2) afforded the title compound (150 mg). 1H NMR: (400 MHz, DMSO-d6): δ 6.38 (d, 1H, J=8.0 Hz), 6.18 (d, 1H, J=2.4 Hz), 5.99 (dd, 1H, J=2.4 and 8.4 Hz), 4.35 (bs, 2H), 3.97 (bs, 2H), 3.66 (m, 4H), 2.81 (m, 4H).
後処理
- filtrationThe reaction mixture was filtered through Celite
- customthe solvent was removed in vacuum
- customPurification by flash chromatography (5% CH3OH/CH2Cl2)
出典と根拠
- ORDレコード
- ord-c325b2725cb747b3a7ec2170d4538f15
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08569511B2
反応ノート
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