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

HRID 726143

반응식

HRID 726143 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 1049Pyridine용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-7b250f591ac24bd79e4f5435df536049
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05708033

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