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Potassium Carbonate → HCID 57872776、化合物

HRID 1664090
ノート
印刷プレビュー

反応式

HRID 1664090 の反応式
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:13]=[C:14](B(O)O)[CH:15]=[C:16]([F:18])[CH:17]=1.C([O-])([O-])=O.[K+].[K+]>C1(C)C=CC=CC=1.O.CCOCC.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:13]=[C:14]([C:2]2[CH:7]=[C:6]([N:8]([CH3:10])[CH3:9])[CH:5]=[CH:4][N:3]=2)[CH:15]=[C:16]([F:18])[CH:17]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 11430Potassium CarbonateHCID 2734338(3,5-Difluorophenyl)boronic acidHCID 110861002-Iodo-4-dimethylaminopyridine

生成物 1

HCID 57872776HCID 57872776、化合物収率 47.4%

試薬・触媒・溶媒 4

HCID 178418397HCID 178418397、化合物触媒
HCID 962
Water
溶媒
HCID 1140Toluene溶媒
HCID 3283Diethyl Ether溶媒

反応条件

温度
90 °C

実験手順

A mixture of 2-iodo-4-dimethylaminopyridine (2.68 g, 10.8 mmol), 3,5-difluorophenylboronic acid (2.56 g, 16.2 mmol) and K2CO3 (6.7 g, 48.6 mmol) in toluene (60 ml) and water (10 ml) were degased 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 afford a brown oil. The following 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 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 obtained residue was then purified by column chromatography (SiO2, EtOAc) to afford 1.2 g (46%) of the titled compound as a colorless oil, which solidify upon standing. The crude compound was purified by column chromatography (SiO2, CHCl3 then CHCl3/MeOH, 97/3) to afford 1 g (40%) of the titled compound as a colorless oil, which solidify upon standing.

後処理

  1. customwere degased 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 afford a brown oil
  10. extractionextracted with 10% HCl solution (3×50 ml)
  11. washThe combined aqueous fractions were washed with Et2O (2×100 ml) and neutralized with concentrated NaOH solution
  12. extractionThe resulting mixture was extracted with EtOAc (4×100 ml)
  13. washthe combined organic fractions were washed with brine (50 ml)
  14. dry with materialdried over MgSO4
  15. filtrationfiltered
  16. customevaporated to dryness
  17. customThe obtained residue was then purified by column chromatography (SiO2, EtOAc)

出典と根拠

ORDレコード
ord-f3a865314a2c40a29afcccc89b0b2796
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08039124B2

反応ノート

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