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Methyl 2-chloropyridine-4-carboxylate → HCID 66731569, 화합물

HRID 1963309
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HRID 1963309 반응식
Cl[C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][N:11]=1)[C:5]([O:7][CH3:8])=[O:6].[Br-].[F:13][C:14]1[CH:21]=[CH:20][C:19]([F:22])=[CH:18][C:15]=1[CH2:16][Zn+]>C1COCC1.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>[F:13][C:14]1[CH:21]=[CH:20][C:19]([F:22])=[CH:18][C:15]=1[CH2:16][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][N:11]=1)[C:5]([O:7][CH3:8])=[O:6]
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참가 물질

5

반응물 2

HCID 2736842Methyl 2-chloropyridine-4-carboxylateHCID 178505810HCID 178505810, 화합물

생성물 1

HCID 66731569HCID 66731569, 화합물수율 79.1%

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

To a solution of methyl 2-chloroisonicotinate (5.6 g, 32.64 mmol) and Pd(PPh3)4 (0.754 g, 0.65 mmol) in anhydrous THF (100 mL) was added (2,5-difluorobenzyl)zinc(II) bromide (0.5 M in THF) (100 mL, 50.00 mmol) dropwise under nitrogen. The reaction mixture was heated at 60° C. for 15 h. The reaction mixture was quenched by addition of methanol (50 mL) and then filtered. The solvent was evaporated under reduced pressure. The residue was dissolved in ethyl acetate and washed with satd NH4Cl solution and brine, then dried. The solvent was evaporated under reduced pressure. The residue was suspended in ethanol, filtered and the solid washed with ethanol. The filtrate was concentrated. The residue was dissolved in MTBE (150 mL), then HCl (4 M in dioxane, (8.15 mL) and MeOH (7.5 mL) were added. The resulting suspension was stirred for 20 min, the solid collected, washed with MTBE (×2) and air dried. The solid was dissolved in DCM (200 mL) and washed with satd NaHCO3. The organic phase was dried using a phase separator and evaporated to yield methyl 2-(2,5-difluorobenzyl)isonicotinate (6.8 g, 79%). MS m/z 264 (M+H)+

후처리

  1. customThe reaction mixture was quenched by addition of methanol (50 mL)
  2. filtrationfiltered
  3. customThe solvent was evaporated under reduced pressure
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washwashed with satd NH4Cl solution and brine
  6. customdried
  7. customThe solvent was evaporated under reduced pressure
  8. filtrationfiltered
  9. washthe solid washed with ethanol
  10. concentrationThe filtrate was concentrated
  11. dissolutionThe residue was dissolved in MTBE (150 mL)
  12. additionHCl (4 M in dioxane, (8.15 mL) and MeOH (7.5 mL) were added
  13. customthe solid collected
  14. washwashed with MTBE (×2) and air
  15. customdried
  16. dissolutionThe solid was dissolved in DCM (200 mL)
  17. washwashed with satd NaHCO3
  18. customThe organic phase was dried
  19. customevaporated

출처 및 근거

ORD 기록
ord-a0d9d95bf2f74599b783e2df21a1afc5
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08415378B2

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