反応式
[CH3:1][NH:2][C:3](=[O:14])[CH2:4][CH2:5][CH:6]([N+:11]([O-])=O)[CH:7]([OH:10])[CH2:8][F:9]>CO.[Ni]>[CH3:1][NH:2][C:3](=[O:14])[CH2:4][CH2:5][CH:6]([NH2:11])[CH:7]([OH:10])[CH2:8][F:9]参加物
4
実験手順
To a solution of 6-fluoro-5-hydroxy-4-nitro-hexanoic acid methylamide (0.325 g, 1.56 mmol) in MeOH (12 mL) was added Raney Ni (about 0.12 g), and the mixture was shaken under H2 (40-45 psi) at room temperature for 18 h. The black mixture was filtered through celite, and the celite was washed with additional MeOH (100 mL). The yellow solution was concentrated to give yellow oil (0.250 g, 90%), which was used without further purification. 1H NMR (CDCl3): 5.68 (br s, NH, 1H), 4.64-4.38 (m, 2H), 3.64-3.49 (m, 1H), 2.90-2.85 (m, 1H), 2.81 (d, J=5.10 Hz, 3H), 2.40-2.29 (m, 2H), 1.97-1.88 (m, 2H); Mass Spectra: ESI: calculated: 178.11. found: MH+ 179.18.
後処理
- filtrationThe black mixture was filtered through celite
- washthe celite was washed with additional MeOH (100 mL)
- concentrationThe yellow solution was concentrated
出典と根拠
- ORDレコード
- ord-0b7d8e7f59b64f14b2c09fbad273ee7f
- 出典データセット
- uspto-grants-2009_03
- 特許番号
- US07504382B2
関連ノート
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