1,5-Dimethyl-3-nitropyridin-2-one → 3-Amino-1,5-dimethyl-1,2-dihydropyridin-2-one
反応式
[CH3:1][N:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([N+:9]([O-])=O)[C:3]1=[O:12]>CO.[Ni]>[NH2:9][C:4]1[C:3](=[O:12])[N:2]([CH3:1])[CH:7]=[C:6]([CH3:8])[CH:5]=1参加物
4
実験手順
A solution of 9.74 g (57.9 mmol) 1,5-dimethyl-3-nitropyridin-2(1H)-one (product from step 199.5), 2 g (57.9 mmol) Raney-Ni in 230 ml methanol was shaken in a duck glass under H2 atmosphere for 16 hours. After that, the mixture was filtered over celite, washed with MeOH, concentrated in vacuum and dried at high vacuum over night to obtain 7.9 g (57.2 mmol, 99% yield) of the title compound as a brownish solid. LCMS: (M+H)=139; tR=0.43 min (LC-MS 6). HPLC: tR=1.22 min (HPLC 8). 1H-NMR (DMSO-d6, 400 MHz) δ ppm 6.67 (m, 1H) 6.30 (m, 1H) 5.05 (bs, 2H) 3.38 (s, 3H) 1.93 (s, 3H).
後処理
- filtrationAfter that, the mixture was filtered over celite
- washwashed with MeOH
- concentrationconcentrated in vacuum
- customdried at high vacuum over night
出典と根拠
- ORDレコード
- ord-7e550b70526e45ccb5acbf160a7af81e
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08969341B2
反応ノート
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