HCID 11458385、化合物 → HCID 21701862、化合物
反応式
[N+:1]([C:4]1[C:9]2[CH2:10][CH2:11][CH2:12][CH2:13][C:14](=O)[C:8]=2[CH:7]=[CH:6][CH:5]=1)([O-])=O.[H][H]>C(O)(=O)C.[Pd]>[C:4]1([NH2:1])[CH:5]=[CH:6][CH:7]=[C:8]2[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][C:9]=12参加物
5
実験手順
A solution of 1-nitro-6,7,8,9-tetrahydro-5H-benzo[7]annulene-5-one (CAS #251554-42-4, 2.5 g, 12 mmol), palladium (413 mg, 10% on carbon, 0.4 mmol) in acetic acid (25 ml) under the hydrogen atmosphere (60 PSI) was heated at 60° C. and stirred at for 16 hours. The mixture was filtered through a layer of diatomaceous earth, washed with methanol and concentrated under reduced pressure to provide the title compound. 1H NMR (CDCl3) δ 1.50-1.69 (m, 4H), 1.75-1.86 (m, 2H), 2.71-2.86 (m, 4H), 5.46 (s, 2H), 7.03-7.12 (m, 3H). MS (M+H)+ m/z 162.
後処理
- filtrationThe mixture was filtered through a layer of diatomaceous earth
- washwashed with methanol
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-25d5bc22a7814628bf4159cc0404bf9a
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08735411B2
反応ノート
読み込み中…