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Sodium Bicarbonate → HCID 21075865, 화합물

HRID 1374157
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HRID 1374157 반응식
FC(F)(F)S(O[C:7]1[CH:8]=[N:9][CH:10]=[C:11]([Cl:13])[CH:12]=1)(=O)=O.B1(B2OC(C)(C)C(C)(C)O2)OC(C)(C)C(C)(C)O1.C([O-])(=O)C.[K+].[F:39][C:40]1[CH:45]=[CH:44][CH:43]=[C:42](I)[C:41]=1[C:47]1[N:48]=[N:49][N:50]([CH3:52])[N:51]=1.C(=O)(O)[O-].[Na+]>CN(C=O)C.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[Cl:13][C:11]1[CH:10]=[N:9][CH:8]=[C:7]([C:42]2[CH:43]=[CH:44][CH:45]=[C:40]([F:39])[C:41]=2[C:47]2[N:48]=[N:49][N:50]([CH3:52])[N:51]=2)[CH:12]=1
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참가 물질

8

반응물 5

HCID 516892Sodium BicarbonateHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 151858705-Chloropyridin-3-yl trifluoromethanesulfonateHCID 161029015-(2-Fluoro-6-iodophenyl)-2-methyl-2H-tetrazole

생성물 1

HCID 21075865HCID 21075865, 화합물

시약·촉매·용매

2
HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)촉매2회HCID 6228Dimethylformamide용매

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온도
80 °C

실험 절차

A mixture of 5-chloropyridin-3-yl trifluoromethanesulfonate (6.00 g, 22.9 mmol), bis(pinacolato)diboron (6.12 g, 24.1 mmol), potassium acetate (6.75 g, 68.8 mmol), and [1,1′-bis-(diphenylphosphino)ferrocene]palladium(II) dichloride (0.60 g, 0.82 mmol) in 30 mL DMF was heated to 80° C. under N2 for 2 hours. The reaction mixture was cooled to room temperature, and 5-(2-fluoro-6-iodophenyl)-2-methyl-2H-tetrazole (4.88 g, 16.1 mmol), sodium bicarbonate (2M, 34.4 mL, 68.8 mmol), and [1,1′-bis(diphenylphosphino)ferrocene]palladium(II) dichloride (0.60 g, 0.82 mmol) were added. The reaction mixture was heated to 80° C. overnight, then cooled to room temperature and partitioned between ethyl acetate and water. The organic extract was washed with water and brine, dried over Na2SO4, filtered and concentrated under vacuum. The residue was subjected to silica gel chromatography eluted with 0–30% ethyl acetate in hexanes to provide 3-chloro-5-[3-fluoro-2-(2-methyl-2H-tetrazol-5-yl)phenyl]pyridine that gave proton NMR spectra consistent with theory and a mass ion (ES+) of 290.11 for M+H+.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. temperatureThe reaction mixture was heated to 80° C. overnight
  3. temperaturecooled to room temperature
  4. custompartitioned between ethyl acetate and water
  5. extractionThe organic extract
  6. washwas washed with water and brine
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated under vacuum
  10. washeluted with 0–30% ethyl acetate in hexanes

출처 및 근거

ORD 기록
ord-e81b485628114c8f8dc3941b4f58b8c8
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07163951B2

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