Hydrochloric Acid → 2-Propenoic acid, 3-(2-chloro-4-fluorophenyl)-

HRID 726143ノート

反応式

HRID 726143 の反応式
[Cl:1][C:2]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:3]=1[CH:4]=O.C(O)(=O)[CH2:12][C:13]([OH:15])=[O:14].N1CCCCC1.Cl>N1C=CC=CC=1.O>[Cl:1][C:2]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:3]=1[CH:4]=[CH:12][C:13]([OH:15])=[O:14]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 867Malonic AcidHCID 8082PiperidineHCID 1450242-Chloro-4-fluorobenzaldehyde

生成物 1

HCID 27250652-Propenoic acid, 3-(2-chloro-4-fluorophenyl)-収率 96%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1049Pyridine溶媒

実験手順

To a mixture of 2-chloro-4-fluorobenzaldehyde (20.0 g, 0.13 mol, Aldrich) and malonic acid (26.2 g, 0.25 mol, Aldrich) in pyridine (100 ml) at 50° C. was added dropwise piperidine (10 ml). After 18 h at 70° C., the mixture was poured into an ice cold solution of concentrated HCl (120 ml) and water (1.5 L). The resulting solid was filtered and washed repeatedly with water to give 24.4 g (96%) of 2-chloro-4-fluoro-cinnamic acid as a white solid: Recrystallization of 1.5 g from acetone:water mixtures gave 1.1 g of 2-chloro-4-fluorocinnamic acid as a white solid: mp 243°-245° C.

後処理

  1. filtrationThe resulting solid was filtered
  2. washwashed repeatedly with water

出典と根拠

ORDレコード
ord-7b250f591ac24bd79e4f5435df536049
出典データセット
uspto-grants-1998_01
特許番号
US05708033

反応ノート

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