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Sodium borohydride → ethyl (2RS,3RS)-2-[3-(1,1-difluoroethyl)benzyl]-3-(4-fluorophenyl)-3-hydroxypropionate

HRID 1610723
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HRID 1610723 반응식
[BH4-].[Na+].[F:3][C:4]([C:7]1[CH:8]=[C:9]([CH:26]=[CH:27][CH:28]=1)[CH2:10][CH:11]([C:17]([C:19]1[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=1)=[O:18])[C:12]([O:14][CH2:15][CH3:16])=[O:13])([F:6])[CH3:5]>CCOCC.[Cl-].[Zn+2].[Cl-]>[F:3][C:4]([C:7]1[CH:8]=[C:9]([CH:26]=[CH:27][CH:28]=1)[CH2:10][CH:11]([CH:17]([C:19]1[CH:20]=[CH:21][C:22]([F:25])=[CH:23][CH:24]=1)[OH:18])[C:12]([O:14][CH2:15][CH3:16])=[O:13])([F:6])[CH3:5]
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참가 물질

5

반응물 2

HCID 4311764Sodium borohydrideHCID 22261820Ethyl 2-[3-(1,1-difluoroethyl)benzyl]-3-(4-fluorophenyl)-3-oxopropionate

생성물 1

HCID 86593306ethyl (2RS,3RS)-2-[3-(1,1-difluoroethyl)benzyl]-3-(4-fluorophenyl)-3-hydroxypropionate수율 87%

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 3283Diethyl Ether용매2회

실험 절차

To a suspension (40 ml) of zinc chloride (5.35 g, 39.2 mmol) in ether was added sodium borohydride (2.97 g, 78.4 mmol) at room temperature, and the mixture was stirred as it was for 2 hrs. Insoluble material was filtered off. To the filtrate was added a solution of ethyl 2-[3-(1,1-difluoroethyl)benzyl]-3-(4-fluorophenyl)-3-oxopropionate (7.16 g, 19.6 mmol) in ether (40 ml), and the mixture was stirred at room temperature for 1.5 hrs. The reaction was quenched with 1N hydrochloric acid, and the mixture was diluted with ethyl acetate and washed with water and saturated brine. The mixture was dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=8:1, 4:1) to give ethyl (2RS,3RS)-2-[3-(1,1-difluoroethyl)benzyl]-3-(4-fluorophenyl)-3-hydroxypropionate (6.24 g, 87%) as a colorless transparent oil.

후처리

  1. filtrationInsoluble material was filtered off
  2. stirringthe mixture was stirred at room temperature for 1.5 hrs
  3. customThe reaction was quenched with 1N hydrochloric acid
  4. additionthe mixture was diluted with ethyl acetate
  5. washwashed with water and saturated brine
  6. dry with materialThe mixture was dried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=8:1, 4:1)

출처 및 근거

ORD 기록
ord-55ec6dcb952746c5aec907c30767b205
출처 데이터셋
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06982348B2

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