3-(2,4-Difluorophenyl)acrylic Acid → 3-(2,4-difluorophenyl)propanoic Acid

HRID 130605

반응식

HRID 130605 반응식
[F:1][C:2]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:3]=1[CH:4]=[CH:5][C:6]([OH:8])=[O:7].[H][H]>O1CCCC1.[Pd]>[F:1][C:2]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:3]=1[CH2:4][CH2:5][C:6]([OH:8])=[O:7]

참가 물질

5

반응물 2

HCID 6035023-(2,4-Difluorophenyl)acrylic AcidHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 49863953-(2,4-difluorophenyl)propanoic Acid수율 98.1%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매

반응 조건

온도
100 °C

실험 절차

105 g of 2,4-difluorocinnamic acid from Example 5 were dissolved in 450 ml of tetrahydrofuran and reacted with 5 g of palladium on active carbon with stirring at 100° C. and a hydrogen pressure of 50 bar. After a constant pressure had been achieved, the mixture was cooled to room temperature, the pressure was released, the palladium catalyst was filtered off and the solvent was removed by distillation. After drying in vacuo, 104.1 g of 3-(2,4-difluorophenyl)-propionic acid (98% of theory; melting point: 100-102° C.) were obtained.

후처리

  1. temperaturethe mixture was cooled to room temperature
  2. filtrationthe palladium catalyst was filtered off
  3. customthe solvent was removed by distillation
  4. customAfter drying in vacuo

출처 및 근거

ORD 기록
ord-a3ee7cc74cbf476d81e3da58a05df9d4
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07381832B2

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