反応式
Br[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[C:15]#[N:16])=[CH:5][CH:4]=1.[CH3:17][O:18][C:19](=[O:25])[C@H:20]([CH:22]([CH3:24])[CH3:23])[NH2:21].[C:26](=[O:29])([O-:28])[O-].[K+].[K+].[I-].[K+]>C(#N)C>[C:19]([OH:25])(=[O:18])[C:26]([OH:28])=[O:29].[CH3:17][O:18][C:19](=[O:25])[C@H:20]([CH:22]([CH3:24])[CH3:23])[NH:21][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[C:15]#[N:16])=[CH:5][CH:4]=1参加物
6
反応条件
- 温度
- 42.5 °C
実験手順
In one of the preferred embodiments 4-bromomethyl-2′-cyanobiphenyl, L-valine methyl ester, potassium carbonate and potassium iodide are taken in acetonitrile. The reaction mixture was stirred at about 40-45° C. for about 3 to 4 hours and the solvent was removed under vacuum. Water and xylene was added to reaction mass and the organic layer was separated. A solution of oxalic acid was added to the organic layer and stirred for about an hour at ambient temperature to give N-[(2′-cyanobiphenyl-4-yl)methyl]-(L)-valine methyl ester oxalate salt.
後処理
- customthe solvent was removed under vacuum
- additionWater and xylene was added to reaction mass
- customthe organic layer was separated
- additionA solution of oxalic acid was added to the organic layer
- stirringstirred for about an hour at ambient temperature
出典と根拠
- ORDレコード
- ord-d17d76d5bf9d49e0bd43c815da86fdef
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07741507B2
関連ノート
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