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

HRID 985536
ノート
印刷プレビュー

反応式

HRID 985536 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[CH:39]=[CH:38][S:37][C:36]=3[C:40]#[N:41])[CH:32]=[CH:33][CH:34]=2)O1>CN(C)C(=O)C.O.C(=O)([O-])O.[Na+]>[CH:11]([C:9]1[CH:8]=[CH:7][N:6]2[C:2]([C:33]3[CH:32]=[C:31]([C:35]4[CH:39]=[CH:38][S:37][C:36]=4[C:40]#[N:41])[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

7

反応物 3

HCID 62657Potassium Phosphate, TribasicHCID 225070883-[3-(4,4,5,5-Tetramethyl-[1,3,2]dioxaborolan-2-yl)phenyl]thiophene-2-carbonitrileHCID 768496803-Bromoimidazo[1,2-A]pyridine-7-carbaldehyde

生成物 1

HCID 99020133-[3-(7-Formylimidazo[1,2-alpha]pyridin 3-yl)phenyl]thiophene-2-carbonitrile収率 68%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 31374Dimethylacetamide溶媒
HCID 516892Sodium Bicarbonate溶媒

反応条件

温度
80 °C

実験手順

3-Bromoimidazo[1,2-α]pyridine-7-carboxaldehyde (1.15 g, 5.16 mmol), potassium phosphate (2.19 g, 10.31 mmol) and 3-[3-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)phenyl]thiophene-2-carbonitrile (2.58 g, 8.26 mmol) were dissolved in N,N-dimethylacetamide (15 ml) and the mixture degassed with N2 for 15 min. Tetrakis(triphenylphosphine)pallidum(0) (0.30 g, 0.26 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 (2×75 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 (1-2%). The solid obtained was triturated with diethyl ether which gave the title compound (1.15 g, 68%) as a white powder. Oxalate salt, white powder. 1H NMR (360 MHz, d6-DMSO) δH 7.30 (1H, dd, J 7 and 1), 7.70-7.88 (4H, m), 8.08 (1H, s), 8.16-8.22 (2H, m), 8.44 (1H, s), 8.78 (1H, d, J 7), 10.05 (1H, s); m /z (ES+) 330 (M++H).

後処理

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

出典と根拠

ORDレコード
ord-a8a221c07de14e5789a0b6fe31606d20
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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