3-[3-fluoro-4-(trifluoromethyl)phenyl]prop-2-enoic Acid → 3-[3-Fluoro-4-(trifluoromethyl)phenyl]propionic acid

HRID 1844040노트

반응식

HRID 1844040 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][C:14]([OH:16])=[O:15])[CH:5]=[CH:6][C:7]=1[C:8]([F:11])([F:10])[F:9]>CO.C(Cl)(Cl)Cl>[F:1][C:2]1[CH:3]=[C:4]([CH2:12][CH2:13][C:14]([OH:16])=[O:15])[CH:5]=[CH:6][C:7]=1[C:8]([F:11])([F:10])[F:9]

참가 물질

4

반응물 1

HCID 27375813-[3-fluoro-4-(trifluoromethyl)phenyl]prop-2-enoic Acid

생성물 1

HCID 467374883-[3-Fluoro-4-(trifluoromethyl)phenyl]propionic acid수율 81.8%

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 6212Chloroform용매

실험 절차

10% NIX was added to a stirred solution of 3-(3-fluoro-4-(trifluoromethyl)phenyl)-acrylic acid (I-77a: 5.5 g, 0.0234 mol) in methanol. The resulting mixture was stirred under hydrogen atmosphere for 4 hours. The reaction was monitored by TLC (5% methanol in CHCl3). The catalyst was filtered through celite bed and the solvent distilled under reduced pressure to afford the crude product. Purification by column chromatography on silica gel (2% methanol in CHCl3) afforded 4.5 g of the product (81.8% yield).

후처리

  1. filtrationThe catalyst was filtered through celite bed
  2. distillationthe solvent distilled under reduced pressure
  3. customto afford the crude product
  4. customPurification by column chromatography on silica gel (2% methanol in CHCl3)

출처 및 근거

ORD 기록
ord-952d023f73f04fedab2c6da7a5e6b182
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946260B2

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