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

HRID 2359324
ノート
印刷プレビュー

反応式

HRID 2359324 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 5

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

生成物 1

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

試薬・触媒・溶媒

5
HCID 6397Chlorotrimethylsilane触媒HCID 78391,2-Dibromoethane触媒HCID 23994Zinc触媒2 回HCID 588388791,3-Bis[2,6-di(propan-2-yl)phenyl]imidazolidin-2-ide;3-chloropyridine;dichloropalladium触媒HCID 8028Tetrahydrofuran溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-42f1bf1861394012932bf6d5969b32ba
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08685977B2

反応ノート

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