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Potassium Phosphate, Tribasic → 3'-(7-Formylimidazo[1,2-alpha]pyridin-3-yl)biphenyl-2-carbonitrile

HRID 985542
ノート
印刷プレビュー

反応式

HRID 985542 の反応式
Br[C:2]1[N:6]2[CH:7]=[CH:8][C:9]([CH:11]=[O:12])=[CH:10][C:5]2=[N:4][CH:3]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].CC1(C)C(C)(C)OB([C:29]2[CH:30]=[C:31]([C:35]3[C:36]([C:41]#[N:42])=[CH:37][CH:38]=[CH:39][CH:40]=3)[CH:32]=[CH:33][CH:34]=2)O1>CN(C)C(=O)C.O.C(=O)([O-])O.[Na+].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>[CH:11]([C:9]1[CH:8]=[CH:7][N:6]2[C:2]([C:33]3[CH:32]=[C:31]([C:35]4[C:36]([C:41]#[N:42])=[CH:37][CH:38]=[CH:39][CH:40]=4)[CH:30]=[CH:29][CH:34]=3)=[CH:3][N:4]=[C:5]2[CH:10]=1)=[O:12]
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 62657Potassium Phosphate, TribasicHCID 112436553'-(4,4,5,5-Tetramethyl-[1,3,2]dioxaborolan-2-yl)biphenyl-2-carbonitrileHCID 768496803-Bromoimidazo[1,2-A]pyridine-7-carbaldehyde

生成物 1

HCID 98583783'-(7-Formylimidazo[1,2-alpha]pyridin-3-yl)biphenyl-2-carbonitrile収率 32.8%

試薬・触媒・溶媒 4

HCID 178418397
HCID 178418397、化合物
触媒
HCID 962Water溶媒
HCID 31374Dimethylacetamide溶媒2 回
HCID 516892Sodium Bicarbonate溶媒

反応条件

温度
80 °C

実験手順

Trifluoromethanesulfonic acid 2′-cyanobiphenyl-3-yl ester (0.55 g, 1.66 mmol), potassium acetate (0.49 g, 4.98 mmol) and bis(pinacolato)diboron (0.55 g, 2.16 mmol) were dissolved in 1,4-dioxane (10 ml) and the mixture degassed with N2 for 15 min. Dichloro[1,1′-bis(diphenylphosphino)ferrocene]palladium(II) dichloromethane adduct (41 mg, 0.05 mmol) and 1,1′-bis(diphenylphosphino)ferrocene (28 mg, 0.05 mmol) were then added and the mixture heated at 85° C. for 18 h. The mixture was cooled to ambient temperature and partitioned between ethyl acetate (150 ml) and water (50 ml). The organic layer was washed with brine (50 ml), dried over anhydrous sodium sulfate and evaporated in vacuo to give 3′-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)biphenyl-2-carbonitrile as a black oil (0.51 g, 100%). This oil was dissolved in sufficient N,N-dimethylacetamide to give a 0.5 M stock solution. 3-Bromoimidazo[1,2-α]pyridine-7-carboxaldehyde (0.70 g, 3.11 mmol), potassium phosphate (0.99 g, 4.67 mmol) and 3′-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)biphenyl-2-carbonitrile (1.80 g, 5.90 mmol) were dissolved in N,N-dimethylacetamide (6 ml) and the mixture degassed with N2 for 15 min. Tetrakis(triphenylphosphine)palladium(0) (0.14 g, 0.12 mmol) was added and the mixture heated at 80° C. for 18 h. The mixture was allowed to cool to room temperature, diluted with water (20 ml) and saturated sodium hydrogencarbonate solution (20 ml), then extracted with ethyl acetate (3×75 ml). The combined organic fractions were washed with brine (40 ml), dried over anhydrous sodium sulfate and evaporated to give a black oil. The oil was purified by silica gel chromatography eluting with dichloromethane and 1% conc. ammonia on a gradient of methanol (1-3%). The solid obtained was triturated with diethyl ether which gave the title compound (0.33 g, 29%) as a yellow powder. 1H NMR (400 MHz, CDCl3) δH 7.41 (1H, dd, J 7 and 1), 7.52 (1H, dt, J 8 and 1), 7.58 (1H, d, J 7), 7.62-7.73 (4H, m), 8.81-8.44 (2H, m), 7.98 (1H, s), 8.18 (1H, d, J 1), 8.63 (1H, d, J 7), 10.03 (1H, s); m/z (ES+) 324 (M++H).

後処理

  1. customto give a 0.5 M stock solution
  2. customthe mixture degassed with N2 for 15 min
  3. temperatureto cool to room temperature
  4. extractionextracted with ethyl acetate (3×75 ml)
  5. washThe combined organic fractions were washed with brine (40 ml)
  6. dry with materialdried over anhydrous sodium sulfate
  7. customevaporated
  8. customto give a black oil
  9. customThe oil was purified by silica gel chromatography
  10. washeluting with dichloromethane and 1% conc. ammonia on a gradient of methanol (1-3%)
  11. customThe solid obtained
  12. customwas triturated with diethyl ether which

出典と根拠

ORDレコード
ord-e95de5684270491989ffe826db05e855
出典データセット
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06872731B2

反応ノート

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