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Sodium hydride → Ethyl 3-(3-chlorophenyl)-3-oxo-2-[4-(2,2,3,3,3-pentafluoropropyl)benzyl]propionate

HRID 1610753
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HRID 1610753 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:8](=[O:15])[CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:5]=[CH:6][CH:7]=1.[H-].[Na+].Br[CH2:19][C:20]1[CH:25]=[CH:24][C:23]([CH2:26][C:27]([F:33])([F:32])[C:28]([F:31])([F:30])[F:29])=[CH:22][CH:21]=1>C(COC)OC>[Cl:1][C:2]1[CH:3]=[C:4]([C:8](=[O:15])[CH:9]([CH2:19][C:20]2[CH:25]=[CH:24][C:23]([CH2:26][C:27]([F:32])([F:33])[C:28]([F:29])([F:30])[F:31])=[CH:22][CH:21]=2)[C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:5]=[CH:6][CH:7]=1
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참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 2757831Ethyl 3-(3-chlorophenyl)-3-oxopropanoateHCID 222623121-(Bromomethyl)-4-(2,2,3,3,3-pentafluoropropyl)benzene

생성물 1

HCID 22262239Ethyl 3-(3-chlorophenyl)-3-oxo-2-[4-(2,2,3,3,3-pentafluoropropyl)benzyl]propionate수율 86%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매2회

실험 절차

A solution of ethyl 3-(3-chlorophenyl)-3-oxopropionate (2.74 g, 12.08 mmol) in dimethoxyethane (30 ml) was ice-cooled, and sodium hydride (60%, 0.49 g, 12.08 mmol) was added, and the mixture was stirred under ice-cooling for 30 min. A solution of 1-(bromomethyl)-4-(2,2,3,3,3-pentafluoropropyl)benzene (3.66 g, 12.08 mmol) in dimethoxyethane (15 ml) was added, and the mixture was stirred overnight at room temperature. After completion of the reaction, the reaction was quenched with 0.5N hydrochloric acid. The mixture was diluted with ethyl acetate, washed with water and saturated brine, dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=15:1, 10:1) to give ethyl 3-(3-chlorophenyl)-3-oxo-2-[4-(2,2,3,3,3-pentafluoropropyl)benzyl]propionate (4.64 g, 86%) as colorless crystals.

후처리

  1. temperaturecooled
  2. temperaturecooling for 30 min
  3. stirringthe mixture was stirred overnight at room temperature
  4. customAfter completion of the reaction
  5. customthe reaction was quenched with 0.5N hydrochloric acid
  6. additionThe mixture was diluted with ethyl acetate
  7. washwashed with water and saturated brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure
  11. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=15:1, 10:1)

출처 및 근거

ORD 기록
ord-12ea1a19cc464a46b07b887b603f6c5a
출처 데이터셋
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06982348B2

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