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Cesium carbonate → 2-(2-(1,5-naphthyridin-2-yl)ethyl)-8-(pyridin-4-yl)-[1,2,4]triazolo[4,3-a]pyridin-3(2H)-one

HRID 1777790
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HRID 1777790 반응식
[N:1]1[C:10]2[C:5](=[N:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH2:11][CH2:12][N:13]1[C:22](=[O:23])[N:16]2[CH:17]=[CH:18][CH:19]=[C:20](Br)[C:15]2=[N:14]1.[N:24]1[CH:29]=[CH:28][C:27](B(O)O)=[CH:26][CH:25]=1.C([O-])([O-])=O.[Cs+].[Cs+]>O1CCOCC1.CCOC(C)=O.CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C>[N:1]1[C:10]2[C:5](=[N:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH2:11][CH2:12][N:13]1[C:22](=[O:23])[N:16]2[CH:17]=[CH:18][CH:19]=[C:20]([C:27]3[CH:28]=[CH:29][N:24]=[CH:25][CH:26]=3)[C:15]2=[N:14]1
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참가 물질

7

반응물 3

HCID 10796Cesium carbonateHCID 2734379(Pyridin-4-yl)boronic acidHCID 715716702-(2-(1,5-naphthyridin-2-yl)ethyl)-8-bromo-[1,2,4]triazolo[4,3-a]pyridin-3(2H)-one

생성물 1

HCID 715717822-(2-(1,5-naphthyridin-2-yl)ethyl)-8-(pyridin-4-yl)-[1,2,4]triazolo[4,3-a]pyridin-3(2H)-one수율 23%

시약·촉매·용매 3

HCID 178418851
HCID 178418851, 화합물
촉매
HCID 8857Ethyl Acetate용매
HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

Triazolopyridinone 10-3 (22 mg, 0.059 mmol) and pyridin-4-ylboronic acid (11 mg, 0.089 mmol) were placed in a microwave vial and dissolved in dioxane (1 mL). To the mixture was added 1 M aq. Cs2CO3 solution (0.12 mL, 0.12 mmol). The mixture was then sparged with N2 gas for 3 min, and bis(tri-tert-butylphosphine)palladium (3.0 mg, 0.006 mmol) was added. The vial was capped and heated at 100° C. under microwave irradiation for 20 min. After cooling, the reaction mixture was diluted with EtOAc (30 mL), washed with water (10 mL) and brine (10 mL), dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by silica gel flash column chromatography (12 g cartridge), eluting with 0-15% MeOH/CH2Cl2. The fractions containing the desired product (10-4) were pooled, and after solvent removal in vacuo, 5.0 mg (23%) of a semisolid were obtained. 1H NMR (300 MHz, CHCl3-d): δ 8.95 (dd, J=4.2, 1.6 Hz, 1H), 8.63 (dd, J=4.8, 1.5 Hz, 2H), 8.37-8.31 (m, 2H), 7.84 (dd, J=6.9, 1.2 Hz, 1H), 7.71 (dd, J=4.8, 1.8 Hz, 2H), 7.63 (dd, J=8.7, 4.2 Hz, 1H), 7.57 (d, J=9.0 Hz, 1H), 7.39 (dd, J=6.9, 1.2 Hz, 1H), 6.64 (t, J=6.9 Hz, 1H), 4.65 (t, J=6.9 Hz, 2H), 3.60 (t, J=6.9 Hz, 2H). HRMS (ES) 369.1443 found (M+H), 369.1461 required.

후처리

  1. customThe mixture was then sparged with N2 gas for 3 min
  2. customThe vial was capped
  3. temperatureAfter cooling
  4. washwashed with water (10 mL) and brine (10 mL)
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by silica gel flash column chromatography (12 g cartridge)
  9. washeluting with 0-15% MeOH/CH2Cl2
  10. additionThe fractions containing the desired product (10-4)
  11. customafter solvent removal in vacuo

출처 및 근거

ORD 기록
ord-f0b6c5263ccd44ab8b386347e6105fa7
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09266881B2

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