Hydrochloric Acid → 4-(p-Chlorocinnamamido)benzoic acid
反応式
[Cl:1][C:2]1[CH:23]=[CH:22][C:5]([CH:6]=[CH:7][C:8]([NH:10][C:11]2[CH:21]=[CH:20][C:14]([C:15]([O:17]CC)=[O:16])=[CH:13][CH:12]=2)=[O:9])=[CH:4][CH:3]=1.[OH-].[K+].C(O)C.Cl>O>[Cl:1][C:2]1[CH:23]=[CH:22][C:5]([CH:6]=[CH:7][C:8]([NH:10][C:11]2[CH:21]=[CH:20][C:14]([C:15]([OH:17])=[O:16])=[CH:13][CH:12]=2)=[O:9])=[CH:4][CH:3]=1参加物
6
実験手順
A solution of 7.1 g. of p-(p-chlorocinnamamido)benzoic acid, ethyl ester and 1.6 g. of potassium hydroxide in 50 ml. of 95% ethanol is stirred at 75° C. overnight. A 25 ml. portion of water and 200 mg. of potassium hydroxide are added, and stirring is continued at 75° C. for 1.5 hours. The mixture is then diluted with 150 ml. of water, adjusted to pH 3 with 37% hydrochloric acid, and the precipitate is collected and dried. The solid is boiled in 100 ml. of methyl cellosolve, cooled, and the solid is collected, washed with ethanol, and dried, giving 5.51 g. of the desired product as a white powder, m.p. 333°-336° C. (dec.).
後処理
- additionThe mixture is then diluted with 150 ml
- customthe precipitate is collected
- customdried
- temperatureof methyl cellosolve, cooled
- customthe solid is collected
- washwashed with ethanol
- customdried
- customgiving 5.51 g
出典と根拠
- ORDレコード
- ord-920d51f5348e4060b245c5a042c489c8
- 出典データセット
- uspto-grants-1985_08
- 特許番号
- US04536346
反応ノート
読み込み中…