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Tetrahydrofuran → 2-Chloro-3-fluoro-4-methyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine

HRID 468932
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HRID 468932 반응식
[Cl:1][C:2]1[C:7]([F:8])=[C:6]([CH3:9])[C:5](I)=[CH:4][N:3]=1.O1CCCC1.[B:16]([O:25][CH:26]([CH3:28])[CH3:27])([O:21][CH:22]([CH3:24])[CH3:23])OC(C)C>>[Cl:1][C:2]1[C:7]([F:8])=[C:6]([CH3:9])[C:5]([B:16]2[O:21][C:22]([CH3:23])([CH3:24])[C:26]([CH3:27])([CH3:28])[O:25]2)=[CH:4][N:3]=1
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참가 물질

4

반응물 3

HCID 8028Tetrahydrofuran2회HCID 21531Triisopropyl borateHCID 102652232-Chloro-3-fluoro-5-iodo-4-methylpyridine

생성물 1

HCID 866749772-Chloro-3-fluoro-4-methyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine

실험 절차

To a −78° C. solution of 2-chloro-3-fluoro-5-iodo-4-methyl-pyridine (498.6 mg; 1.837 mmol) in tetrahydrofuran (6.0 mL; 74 mmol) was added isopropylmagnesium chloride lithium chloride complex (1.3 mol/L) in THF (5.8 mL; 7.5 mmol). The reaction mixture was warmed to room temperature and stirred for 2 hours. The mixture was then re-cooled to −78° C. and triisopropyl borate (2.20 mL; 9.34 mmol) was added. The reaction mixture was stirred at room temperature for 18 hours. The reaction mixture was quenched with a few drops of saturated aqueous ammonium chloride solution, and then a few drops of saturated aqueous sodium carbonate solution were added to cleave the boronate ester. The reaction mixture was dried over magnesium sulfate to afford the boronic acid as a THF solution. To this mixture was added pinacol (3.8865 g; 32.230 mmol), and the mixture was then heated at 40° C. for 24 hours. The reaction mixture was concentrated, absorbed onto silica gel and purified by flash chromatography (40 g silica, solvent gradient: 0-50% ethyl acetate in heptane) to yield 0.2622 g (53%) of the title compound. LCMS (ESI): M+H=272.2; 1H NMR (400 MHz, DMSO) δ 8.30 (s, 1H), 2.47 (d, J=2.3 Hz, 3H), 1.32 (s, 12H).

후처리

  1. temperatureThe mixture was then re-cooled to −78° C.
  2. stirringThe reaction mixture was stirred at room temperature for 18 hours
  3. customThe reaction mixture was quenched with a few drops of saturated aqueous ammonium chloride solution
  4. additiona few drops of saturated aqueous sodium carbonate solution were added
  5. dry with materialThe reaction mixture was dried over magnesium sulfate

출처 및 근거

ORD 기록
ord-9cb0adbfbbee42229251c2e1eb7fb43b
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08623889B2

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