Hydrochloric Acid → 4-(p-Chlorocinnamamido)benzoic acid

HRID 485247ノート

反応式

HRID 485247 の反応式
[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

  1. additionThe mixture is then diluted with 150 ml
  2. customthe precipitate is collected
  3. customdried
  4. temperatureof methyl cellosolve, cooled
  5. customthe solid is collected
  6. washwashed with ethanol
  7. customdried
  8. 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

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