7-Amino-2-methyl-1,2,3,4-tetrahydroquinoline → 2-Methylquinolin-7-amine
反応式
[NH2:1][C:2]1[CH:11]=[C:10]2[C:5]([CH2:6][CH2:7][CH:8]([CH3:12])[NH:9]2)=[CH:4][CH:3]=1>C1(C)C(C)=CC=CC=1.[Pd]>[NH2:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][C:8]([CH3:12])=[N:9]2)=[CH:4][CH:3]=1参加物
4
実験手順
A mixture of 7-amino-2-methyl-1,2,3,4-tetrahydroquinoline (D65) (86 mg) and wet 10% palladium/charcoal (25 mg) in xylene (20 ml) was heated at reflux for 3.5 h. After cooling to room temperature the catalyst was removed via filtration and washed with further xylene. Evaporation of the combined filtrate and washings gave the title compound as a crude off-white solid (87 mg) which was used in the next step without further purification. 1H NMR (400 MHz, CDCl3) δ (ppm): 7.87 (d, 1H), 7.56 (d, 1H), 7.14 (d, 1H), 7.03 (d, 1H), 6.91 (dd, 1H), 4.02 (br, 2H), 2.67 (s, 3H).
後処理
- temperaturewas heated
- temperatureat reflux for 3.5 h
- customwas removed via filtration
- washwashed with further xylene
- customEvaporation of the combined filtrate and washings
出典と根拠
- ORDレコード
- ord-5d6e37a89b3c45379690756bddf6c78f
- 出典データセット
- uspto-grants-2009_05
- 特許番号
- US07538121B2
反応ノート
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