反応式
[N+]([C:4]1[CH:11]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:9]=[CH:8][C:5]=1[C:6]#[N:7])([O-])=O.[CH3:16][O-:17].[Na+].O>CO>[CH3:16][O:17][C:4]1[CH:11]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:9]=[CH:8][C:5]=1[C:6]#[N:7]参加物
5
実験手順
To a solution of 2-nitro-4-(trifluoromethyl)benzonitrile (22.48 g, 104 mmol) in anhydrous methanol (110 ml) was added dropwise 25% sodium methoxide in methanol (24.72 ml, 114.4 mmol), and the resulting mixture stirred at room temperature for 1 hour. Water (110 ml) was added and the resulting solids collected by filtration. The solids were dissolved in DCM (150 ml), washed with sat NaCl (75 ml), dried over Na2SO4, filtered and evaporated to give the title compound (19 g, 91%) as a white solid.
後処理
- filtrationthe resulting solids collected by filtration
- dissolutionThe solids were dissolved in DCM (150 ml)
- washwashed with sat NaCl (75 ml)
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated
出典と根拠
- ORDレコード
- ord-c429fac802f345ae93bd22b24c07a7e3
- 出典データセット
- uspto-grants-2007_10
- 特許番号
- US07285563B2
関連ノート
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