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Sodium Carbonate → 5-(1-Isopropyl-6-oxo-1,6-dihydropyridin-3-yl)thiophene-2-carbaldehyde

HRID 1497477
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HRID 1497477 반응식
I[C:2]1[CH:3]=[CH:4][C:5](=[O:11])[N:6]([CH:8]([CH3:10])[CH3:9])[CH:7]=1.[CH:12]([C:14]1[S:18][C:17](B(O)O)=[CH:16][CH:15]=1)=[O:13].C([O-])([O-])=O.[Na+].[Na+]>C1(C)C=CC=CC=1.C(O)C.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>[CH:8]([N:6]1[C:5](=[O:11])[CH:4]=[CH:3][C:2]([C:17]2[S:18][C:14]([CH:12]=[O:13])=[CH:15][CH:16]=2)=[CH:7]1)([CH3:10])[CH3:9]
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7

반응물 3

HCID 10340Sodium CarbonateHCID 27734305-Formyl-2-thiopheneboronic acidHCID 595418575-iodo-1-isopropylpyridin-2(1H)-one

생성물 1

HCID 866806355-(1-Isopropyl-6-oxo-1,6-dihydropyridin-3-yl)thiophene-2-carbaldehyde수율 53.5%

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매
HCID 702
Ethanol
용매
HCID 1140Toluene용매

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온도
100 °C

실험 절차

To a stirred solution of 5-iodo-1-isopropylpyridin-2(1H)-one (0.41 g, 1.55 mmol) in toluene (5 mL) and ethanol (2 mL) was added 5-formylthiophen-2-yl boronic acid (0.289 g, 1.87 mmol), 2M Na2CO3 (0.495 g, 4.67 mmol), and Pd(PPh3)4 (0.09 g, 0.07 mmol). The mixture was purged with argon and heated at 100° C. for about 2 h. The mixture was concentrated, diluted with water (50 mL), and extracted with ethyl acetate (2×200 mL). The combined organic extracts were washed with brine solution (20 mL), dried over Na2SO4 and concentrated under vacuum to obtain crude product. The crude product was purified by flash chromatography (silica gel, 60-120μ) using 20% ethyl acetate in hexane as eluent to afford 5-(1-isopropyl-6-oxo-1,6-dihydropyridin-3-yl)thiophene-2-carbaldehyde as an off-white solid (0.205 g, 53.3% yield). 1H NMR (400 MHz, DMSO-d6): δ 8.18 (s, 1H), 7.99 (d, 1H), 7.78 (d, 1H), 7.62 (d, 1H), 7.58 (d, 1H), 7.53 (d, 1H), 5.08-5.01 (m, 1H), 1.21 (t, 6H), LC-MS m/z calcd for [M+H]+ 248.07. found 248.1.

후처리

  1. customThe mixture was purged with argon
  2. concentrationThe mixture was concentrated
  3. additiondiluted with water (50 mL)
  4. extractionextracted with ethyl acetate (2×200 mL)
  5. washThe combined organic extracts were washed with brine solution (20 mL)
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated under vacuum
  8. customto obtain crude product
  9. customThe crude product was purified by flash chromatography (silica gel, 60-120μ)

출처 및 근거

ORD 기록
ord-9c874faa0f8f4d088ca89cee9841679f
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09199975B2

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