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Lithium Chloride → 3-(2-Pyridyl)-phenyl acetic acid methyl ester

HRID 1058572
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HRID 1058572 반응식
Br[C:2]1[CH:3]=[C:4]([CH2:8][C:9]([O:11][CH3:12])=[O:10])[CH:5]=[CH:6][CH:7]=1.FC(F)(F)S(O[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=1)(=O)=O.[Cl-].[Li+].C[Sn](C)C.C[Sn](C)C.[F-].[K+].CCOC(C)=O>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O1CCOCC1>[CH3:12][O:11][C:9](=[O:10])[CH2:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=2)[CH:3]=1
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참가 물질

8

반응물 5

HCID 433294Lithium ChlorideHCID 39476262-Pyridyl TrifluoromethanesulfonateHCID 6327618HexamethylditinHCID 11746402Methyl 2-(3-bromophenyl)acetateHCID 131723761HCID 131723761, 화합물

생성물 1

HCID 543647723-(2-Pyridyl)-phenyl acetic acid methyl ester수율 48%

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 312751,4-Dioxane용매

실험 절차

Methyl 3-bromophenylacetate (25 g, 0.109 mol), 2-(trifluoro-methylsulfonyloxy)-pyridine (24.8 g, 0.109 mol), anhydrous lithium chloride (13.89 g, 0.3275 mol), and tetrakis(triphenylphosphine)palladium (6.31 g, 0.0055 mol) were combined, followed by hexamethylditin (35.8 g, 0.109 mol) and anhydrous dioxane (300 ml). The mixture was stirred at reflux for 16h, cooled, and poured into 1:1 saturated KF-EtOAc (1.6 L). The mixture was stirred at RT for 2 h, filtered, and the filtrate was washed with saturated aqueous NaHCO3 (200 ml) and with brine (200 ml), dried (MgSO4), and concentrated in vacuo to give a brown oil. The residue was flash chromatographed (silica gel, 1:4 EtOAc:hexane) to give the title compound as a yellow oil (11.9 g. 48% yield): MS(ES+) 228.1 (MH+). cf. Tetrahedron Letters, 1995, 36, 9085-9088

후처리

  1. temperaturecooled
  2. stirringThe mixture was stirred at RT for 2 h
  3. filtrationfiltered
  4. washthe filtrate was washed with saturated aqueous NaHCO3 (200 ml) and with brine (200 ml)
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo
  7. customto give a brown oil
  8. customchromatographed (silica gel, 1:4 EtOAc:hexane)

출처 및 근거

ORD 기록
ord-9432548c5cd54f3486a150f974b20d41
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06518267B1

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