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Potassium Carbonate → 2-(2,4-Difluorophenyl)-N,N-dimethylpyridin-4-amine

HRID 874090
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HRID 874090 반응식
I[C:2]1[CH:7]=[C:6]([N:8]([CH3:10])[CH3:9])[CH:5]=[CH:4][N:3]=1.[F:11][C:12]1[CH:17]=[C:16]([F:18])[CH:15]=[CH:14][C:13]=1B(O)O.C([O-])([O-])=O.[K+].[K+]>C1(C)C=CC=CC=1.O.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:11][C:12]1[CH:17]=[C:16]([F:18])[CH:15]=[CH:14][C:13]=1[C:2]1[CH:7]=[C:6]([N:8]([CH3:10])[CH3:9])[CH:5]=[CH:4][N:3]=1
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참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 27343342,4-Difluorophenylboronic acidHCID 110861002-Iodo-4-dimethylaminopyridine

생성물 1

HCID 208073522-(2,4-Difluorophenyl)-N,N-dimethylpyridin-4-amine수율 78.3%

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매
HCID 962
Water
용매
HCID 1140Toluene용매

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온도
90 °C

실험 절차

A mixture of 2-iodo-4-dimethylaminopyridine (3 g, 12 mmol), 2,4-difluorophenylboronic acid (2.3 g, 14.5 mmol) and K2CO3 (6 g 43.5 mmol) in toluene (60 ml) and water (10 ml) were degassed with nitrogen for 15 minutes. Pd(PPh3)4 (800 mg, 0.66 mmol) was added and the resulting mixture was heated to 90° C. for 48 hours under nitrogen. After being cooled to room temperature, the aqueous phase was separated and extracted with EtOAc (3×100 ml). The combined organic fractions were washed with brine, dried over MgSO4, filtered and evaporated. To further purify the compound the so-obtained oil was dissolved in Et2O and extracted with 10% HCl solution (3×50 ml). The combined aqueous fractions were washed with Et2O (2×100 ml) and neutralized with concentrated NaOH aqueous solution. The resulting mixture was extracted with EtOAc (4×100 ml), the combined organic fractions were washed with brine (50 ml), dried over MgSO4, filtered and evaporated to dryness. The crude compound was purified by column chromatography (SiO2, CHCl3 then CHCl3/MeOH, 97/3) to afford 2.2 g (78%) of the titled compound as slightly yellow oil which solidified upon standing.

후처리

  1. customwere degassed with nitrogen for 15 minutes
  2. temperatureAfter being cooled to room temperature
  3. customthe aqueous phase was separated
  4. extractionextracted with EtOAc (3×100 ml)
  5. washThe combined organic fractions were washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customevaporated
  9. customTo further purify the compound the so-obtained oil
  10. dissolutionwas dissolved in Et2O
  11. extractionextracted with 10% HCl solution (3×50 ml)
  12. washThe combined aqueous fractions were washed with Et2O (2×100 ml) and neutralized with concentrated NaOH aqueous solution
  13. extractionThe resulting mixture was extracted with EtOAc (4×100 ml)
  14. washthe combined organic fractions were washed with brine (50 ml)
  15. dry with materialdried over MgSO4
  16. filtrationfiltered
  17. customevaporated to dryness
  18. customThe crude compound was purified by column chromatography (SiO2, CHCl3

출처 및 근거

ORD 기록
ord-49f98f7020db42a2b4ac54aca209e592
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08980440B2

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