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2,2'-Bipyridine → (E)-ethyl 4-(3-(3,5-dichlorophenyl)-4,4,4-trifluorobut-1-enyl)-2-methylbenzoate

HRID 587667
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HRID 587667 반응식
[CH3:1][C:2]1[CH:12]=[C:11]([CH:13]=[CH2:14])[CH:10]=[CH:9][C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5].Br[CH:16]([C:21]1[CH:26]=[C:25]([Cl:27])[CH:24]=[C:23]([Cl:28])[CH:22]=1)[C:17]([F:20])([F:19])[F:18].N1C=CC=CC=1C1C=CC=CN=1>ClC1C=CC=CC=1Cl.Cl[Cu]>[Cl:27][C:25]1[CH:26]=[C:21]([CH:16]([C:17]([F:20])([F:18])[F:19])/[CH:14]=[CH:13]/[C:11]2[CH:10]=[CH:9][C:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])=[C:2]([CH3:1])[CH:12]=2)[CH:22]=[C:23]([Cl:28])[CH:24]=1
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6

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HCID 14742,2'-BipyridineHCID 58390837Ethyl 2-methyl-4-vinylbenzoateHCID 866751181-(1-Bromo-2,2,2-trifluoroethyl)-3,5-dichlorobenzene

생성물 1

HCID 86675123(E)-ethyl 4-(3-(3,5-dichlorophenyl)-4,4,4-trifluorobut-1-enyl)-2-methylbenzoate수율 40%

시약·촉매·용매 2

HCID 62652Cuprous chloride촉매
HCID 7239
1,2-Dichlorobenzene
용매

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온도
180 °C

실험 절차

To a stirred solution of ethyl 2-methyl-4-vinylbenzoate (2.0 g, 10.5 mmol) in 1,2-dichlorobenzene (25 mL) were added 1-(1-bromo-2,2,2-trifluoroethyl)-3,5-dichlorobenzene (6.44 g, 21.0 mmol), CuCl (208 mg, 21 mmol) and 2,2bipyridyl (0.65 g, 4.1 mmol). The reaction mixture was degassed with argon for 30 min and then stirred at 180° C. for 24 h. After the reaction was deemed complete by TLC, the reaction mixture was cooled to 25° C. and filtered, and the filtrate was concentrated under reduced pressure. Purification by flash chromatography (SiO2, 100-200 mesh; eluting with 25-30% EtOAc in petroleum ether) afforded the title compound as a solid (1.7 g, 40%): 1H NMR (400 MHz, CDCl3) δ 7.91 (d, J =8.0 Hz, 1H), 7.37 (m, 1H), 7.27-7.24 (m, 4H), 6.59 (d, J=16.0 Hz, 1H), 6.59 (dd, J=16.0, 8.0 Hz, 1H), 4.38 (q, J=7.2 Hz, 2H), 4.08 (m, 1H), 2.62 (s, 3H), 1.42 (t, J=7.2 Hz, 3H); ESIMS m/z 415.06 ([M−H]−); IR (thin film) 1717, 1255, 1114 cm−1.

후처리

  1. customThe reaction mixture was degassed with argon for 30 min
  2. temperaturethe reaction mixture was cooled to 25° C.
  3. filtrationfiltered
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customPurification
  6. washby flash chromatography (SiO2, 100-200 mesh; eluting with 25-30% EtOAc in petroleum ether)

출처 및 근거

ORD 기록
ord-24131f4e87ea477888061b2f017277e4
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09226501B2

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