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Ammonium Chloride → Ethyl 4-[3-(trifluoromethoxy)benzyl]benzoate

HRID 2359324
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HRID 2359324 반응식
[Cl-].[Li+].Br[CH2:4][C:5]1[CH:15]=[CH:14][C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:7][CH:6]=1.[F:16][C:17]([F:27])([F:26])[O:18][C:19]1[CH:20]=[C:21](Br)[CH:22]=[CH:23][CH:24]=1.CC(C1C=CC=C(C(C)C)C=1N1[C-]=[N+](C2C(C(C)C)=CC=CC=2C(C)C)CC1)C.[Cl-].[NH4+]>[Zn].CC(C1C=CC=C(C(C)C)C=1N1[CH-]N(C2C(C(C)C)=CC=CC=2C(C)C)CC1)C.C1C=NC=C(Cl)C=1.Cl[Pd]Cl.BrCCBr.C[Si](Cl)(C)C.C1COCC1>[F:16][C:17]([F:26])([F:27])[O:18][C:19]1[CH:24]=[C:23]([CH:22]=[CH:21][CH:20]=1)[CH2:4][C:5]1[CH:15]=[CH:14][C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:7][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 5

HCID 25517Ammonium ChlorideHCID 433294Lithium ChlorideHCID 5199641-Bromo-3-(trifluoromethoxy)benzeneHCID 954261Ethyl 4-(bromomethyl)benzoateHCID 10883669SIPr

생성물 1

HCID 58046326Ethyl 4-[3-(trifluoromethoxy)benzyl]benzoate수율 101.7%

시약·촉매·용매

5
HCID 6397Chlorotrimethylsilane촉매HCID 78391,2-Dibromoethane촉매HCID 23994Zinc촉매2회HCID 588388791,3-Bis[2,6-di(propan-2-yl)phenyl]imidazolidin-2-ide;3-chloropyridine;dichloropalladium촉매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of zinc (807 mg, 12.3 mmol) and lithium chloride (523 mg, 12.3 mmol) under argon was warmed for 10 minutes using a hot air gun, allowed to cool and then anhydrous THF (50 mL) added. The zinc was activated by treatment with 1,2-dibromoethane (39 mg, 0.21 mmol) and TMSCl (4.3 mg, 0.04 mmol). To the resulting mixture at 25° C. was added ethyl 4-(bromomethyl)benzoate (1.0 g, 4.15 mmol) and the mixture stirred for 15 minutes. 3-(Trifluoromethoxy)bromobenzene (694 mg, 2.88 mmol) was added, followed by (1,3-bis(2,6-diisopropylphenyl)imidazolidene)(3-chloropyridyl)palladium(II) dichloride [PEPPSI™-SIPr] (28 mg, 0.04 mmol) and the mixture stirred at 25° C. for 1 hour. Saturated ammonium chloride solution was added and the crude product extracted with ether. The ether extract was washed with brine, dried over Na2SO4 and the solvent evaporated in vacuo. The crude product was purified by silica gel column chromatography eluting with 7:3 hexane:ethyl acetate to afford the title compound (950 mg, 71%).

후처리

  1. temperaturewas warmed for 10 minutes
  2. temperatureto cool
  3. stirringthe mixture stirred at 25° C. for 1 hour
  4. extractionthe crude product extracted with ether
  5. extractionThe ether extract
  6. washwas washed with brine
  7. dry with materialdried over Na2SO4
  8. customthe solvent evaporated in vacuo
  9. customThe crude product was purified by silica gel column chromatography
  10. washeluting with 7:3 hexane

출처 및 근거

ORD 기록
ord-42f1bf1861394012932bf6d5969b32ba
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08685977B2

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