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Acetate → HCID 89781946, 화합물

HRID 1055918
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HRID 1055918 반응식
C([Sn](CCCC)(CCCC)[C:6]([O:8]CC)=[CH2:7])CCC.Br[C:20]1[CH:21]=[CH:22][CH:23]=[C:24]2[C:29]=1[N:28]=[C:27]([C:30]([O:32][CH3:33])=[O:31])[CH:26]=[CH:25]2.C(OC=C)=C.C([O-])(=O)C>C1COCC1.Cl.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.CCOC(C)=O.C1(C)C=CC=CC=1>[C:6]([C:20]1[CH:21]=[CH:22][CH:23]=[C:24]2[C:29]=1[N:28]=[C:27]([C:30]([O:32][CH3:33])=[O:31])[CH:26]=[CH:25]2)(=[O:8])[CH3:7]
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참가 물질

10

반응물 4

HCID 175AcetateHCID 8024Vinyl etherHCID 619414Stannane, tributyl(1-ethoxyethenyl)-HCID 58567110Methyl 8-bromoquinoline-2-carboxylate

생성물 1

HCID 89781946HCID 89781946, 화합물수율 82.1%

시약·촉매·용매 5

HCID 313Hydrochloric Acid촉매
HCID 178418397HCID 178418397, 화합물촉매
HCID 1140Toluene용매
HCID 8028Tetrahydrofuran용매
HCID 8857Ethyl Acetate용매

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온도
100 °C

실험 절차

A mixture of Pd(PPh3)4 (608 mg, 0.53 mmol), tributyl(1-ethoxyvinyl)tin (3.91 mL, 11.57 mmol), methyl 8-bromoquinoline-2-carboxylate (2.80 g, 10.52 mmol), and toluene (50 mL) was heated under argon at 100° C. for 18 h. The mixture was then concentrated under reduced pressure and adsorbed onto silica gel. Column chromatography (silica gel, 10-100% EtOAc in hexanes) afforded a mixture of vinyl ether (M+1=258.0) and the desired acetate. This mixture was dissolved in THF (40 mL), the solution was cooled to 0° C., 10 drops of 1N HCl were added, and the solution was stirred at 0° C. for 5 min. EtOAc (100 mL) was added and the resulting solution was washed successively with 1N NaOH (20 mL), water (40 mL) and brine (40 mL). Significant product remained in the aq. layer and was extracted with 25% IPA in CHCl3. The combined organic layers were dried over MgSO4, filtered, and concentrated to give methyl 8-acetylquinoline-2-carboxylate (1.98 g, 8.64 mmol, 82% yield) as a tan solid: 1H NMR (400 MHz, DMSO-d6) δ ppm 8.69 (d, J=8.4 Hz, 1H), 8.27 (dd, J=8.2, 1.4 Hz, 1H), 8.20 (d, J=8.4 Hz, 1H), 8.00 (dd, J=7.2, 1.4 Hz, 1H), 7.79-7.86 (m, 1H), 3.98 (s, 3H), 2.92 (s, 3H). m/z (ESI, +ve ion) 230.0 (M+H)+.

후처리

  1. concentrationThe mixture was then concentrated under reduced pressure
  2. customColumn chromatography (silica gel, 10-100% EtOAc in hexanes) afforded
  3. temperaturethe solution was cooled to 0° C.
  4. washthe resulting solution was washed successively with 1N NaOH (20 mL), water (40 mL) and brine (40 mL)
  5. extractionwas extracted with 25% IPA in CHCl3
  6. dry with materialThe combined organic layers were dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-cfc5e650ac334339ac860a4b28eda408
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394297B2

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