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Tributylvinyltin → Ethyl 5-(pyridin-2-yl)-4-vinylisoxazole-3-carboxylate

HRID 1951948
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HRID 1951948 반응식
Br[C:2]1[C:3]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[N:4][O:5][C:6]=1[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=1.[CH2:18]([Sn](CCCC)(CCCC)C=C)[CH2:19]CC>O1CCOCC1.C(OCC)(=O)C.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.F[P-](F)(F)(F)(F)F.C([N+]1C=CN(C)C=1)CCC>[N:8]1[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=1[C:6]1[O:5][N:4]=[C:3]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:2]=1[CH:18]=[CH2:19]
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참가 물질

7

반응물 2

HCID 81998TributylvinyltinHCID 23006245Ethyl 4-bromo-5-(pyridin-2-yl)isoxazole-3-carboxylate

생성물 1

HCID 58062830Ethyl 5-(pyridin-2-yl)-4-vinylisoxazole-3-carboxylate수율 414.3%

시약·촉매·용매 4

HCID 27341741-Butyl-3-methylimidazolium hexafluorophosphate촉매HCID 178418476HCID 178418476, 화합물
촉매
HCID 8857Ethyl Acetate용매
HCID 312751,4-Dioxane용매

실험 절차

A solution of ethyl 4-bromo-5-(pyridin-2-yl)isoxazole-3-carboxylate (2-C) (170 mg, 0.572 mmol), tributyl(vinyl)tin (0.504 mL, 1.72 mmol), dichlorobis(triphenylphosphine)-palladium(II) (24.1 mg, 0.034 mmol), and 1-butyl-3-methylimidazolium hexafluorophosphate (0.012 mL, 0.057 mmol) in dioxane (3 mL) was heated to 170° C. via microwave for 120 minutes. The reaction mixture was diluted with ethyl acetate (50 mL), washed with water (10 mL), washed with brine (10 mL), and dried over anhydrous sodium sulfate. Concentration gave a crude product which was purified by silica gel chromatography with hexanes/ethyl acetate (4/1) to give ethyl 5-(pyridin-2-yl)-4-vinylisoxazole-3-carboxylate (60 mg, 2.37 mmol, 41% yield). The compound had an HPLC retention time=2.80 min.—Column: YMC S5 COMBISCREEN® 4.6×50 mm; Gradient time: 4 min; Flow rate=4 ml/min; Solvent A=10% MeOH—90% Water—0.2% H3PO4; Solvent B=90% MeOH—10% water—0.2% H3PO4; Start % B=0; Final % B=100. LC-MS: M+1=245.2. 1H NMR (400 MHz, MeOD) δ ppm 1.42 (t, 3H), 4.47 (q, J=7.19 Hz, 2H), 5.49 (dd, J=11.80, 1.25 Hz, 1H), 5.85 (dd, J=18.07, 1.51 Hz, 1H), 7.26 (dd, J=18.07, 11.80 Hz, 1H), 7.51 (ddd, J=7.03, 5.02, 1.76 Hz, 1H), 7.93-8.02 (m, 2H), and 8.72-8.75 (m, 1H).

후처리

  1. washwashed with water (10 mL)
  2. washwashed with brine (10 mL)
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationConcentration
  5. customgave a crude product which
  6. customwas purified by silica gel chromatography with hexanes/ethyl acetate (4/1)

출처 및 근거

ORD 기록
ord-296c276f8eb846f78d66144819e89441
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08404672B2

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