6-Fluoro-5-Hydroxy-4-Nitro-Hexanoic Acid Methylamide → HCID 86625111、化合物

HRID 1784339

反応式

HRID 1784339 の反応式
[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

  1. filtrationThe black mixture was filtered through celite
  2. washthe celite was washed with additional MeOH (100 mL)
  3. 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

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