Carbon Dioxide → p-(2-Chlorophenyl)cinnamic acid

HRID 1659064

反応式

HRID 1659064 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:15]=[CH:14][C:11]([CH:12]=O)=[CH:10][CH:9]=1.C(O)(=O)[CH2:17][C:18]([OH:20])=[O:19].N1CCCCC1.C(=O)=O.Cl>N1C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:15]=[CH:14][C:11]([CH:12]=[CH:17][C:18]([OH:20])=[O:19])=[CH:10][CH:9]=1

参加物

7

反応物 5

HCID 280Carbon DioxideHCID 313Hydrochloric AcidHCID 867Malonic AcidHCID 8082PiperidineHCID 13944002'-Chloro[1,1'-biphenyl]-4-carbaldehyde

生成物 1

HCID 54534814p-(2-Chlorophenyl)cinnamic acid

試薬・触媒・溶媒 1

HCID 1049Pyridine触媒

実験手順

A mixture of 21.6 g. (0.1 mole) of 4-(2'-chlorophenyl)benzaldehyde is heated on a steam bath with 13.2 g. of malonic acid and 95 ml. of pyridine containing 5 drops of piperidine. The mixture is heated for four hours until the liberation of carbon dioxide ceases. The cooled mixture is poured into a mixture of 110 ml. concentrated hydrochloric acid and 500 ml. of ice water. The solid which separates is filtered, washed and 15 ml. portions of cold water and then resuspended in 200 ml. of cold water, filtered, washed with cold water and dried at 40°C. The residue is then recrystallized from ethanol to obtain 4-(2'-chlorophenyl)cinnamic acid.

後処理

  1. additionA mixture of 21.6 g
  2. additionThe cooled mixture is poured into a mixture of 110 ml
  3. filtrationThe solid which separates is filtered
  4. washwashed
  5. filtrationof cold water, filtered
  6. washwashed with cold water
  7. customdried at 40°C
  8. customThe residue is then recrystallized from ethanol

出典と根拠

ORDレコード
ord-892152934a76453b9e213d4fb110d525
出典データセット
uspto-grants-1976_06
特許番号
US03966801

関連ノート

読み込み中…