Bromine → HCID 20386067、化合物
反応式
[C:1]([CH2:3][C:4]1[CH:14]=[CH:13][C:7]([CH2:8][CH2:9]C(O)=O)=[CH:6][CH:5]=1)#[N:2].[Br:15]Br>C(Cl)(Cl)(Cl)Cl>[Br:15][CH2:9][CH2:8][C:7]1[CH:13]=[CH:14][C:4]([CH2:3][C:1]#[N:2])=[CH:5][CH:6]=1参加物
4
実験手順
A mixture of p-cyanomethylhydrocinnamic acid (18.9 g., 0.1 mole), red mercuric oxide (17.2 g., 0.08 mole), and carbon tetrachloride (180 ml.) is stirred at room temperature while bromine (16.0 g., 0.1 mole) is added dropwise during 40 minutes. The resulting mixture is heated at reflux for 1 hour. The mixture is then cooled, filtered, washed with dilute hydrochloric acid and water, and dried over magnesium sulfate. The solution is evaporated to leave the product as a yellow residual oil. It is purified by column chromatography on silica gel with benzene elution.
後処理
- additionis added dropwise during 40 minutes
- temperatureThe resulting mixture is heated
- temperatureat reflux for 1 hour
- temperatureThe mixture is then cooled
- filtrationfiltered
- washwashed with dilute hydrochloric acid and water
- dry with materialdried over magnesium sulfate
- customThe solution is evaporated
出典と根拠
- ORDレコード
- ord-ace078609a414e19a76a0649735888b0
- 出典データセット
- uspto-grants-1979_04
- 特許番号
- US04150235
反応ノート
読み込み中…