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Potassium Phosphate, Tribasic → HCID 10110424、化合物

HRID 895148
ノート
印刷プレビュー

反応式

HRID 895148 の反応式
Br[C:2]1[N:6]2[CH:7]=[N:8][C:9]([C:11]([F:14])([F:13])[F:12])=[CH:10][C:5]2=[N:4][CH:3]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].[F:23][C:24]1[CH:29]=[CH:28][C:27](B2OC(C)(C)C(C)(C)O2)=[CH:26][C:25]=1[C:39]1[C:40]([C:45]#[N:46])=[CH:41][CH:42]=[CH:43][CH:44]=1>CN(C)C(=O)C.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:23][C:24]1[CH:29]=[CH:28][C:27]([C:2]2[N:6]3[CH:7]=[N:8][C:9]([C:11]([F:14])([F:13])[F:12])=[CH:10][C:5]3=[N:4][CH:3]=2)=[CH:26][C:25]=1[C:39]1[C:40]([C:45]#[N:46])=[CH:41][CH:42]=[CH:43][CH:44]=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

6

反応物 3

HCID 62657Potassium Phosphate, TribasicHCID 117716472′-Fluoro-5′-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)[1,1′-biphenyl]-2-carbonitrileHCID 22385760HCID 22385760、化合物

生成物 1

HCID 10110424HCID 10110424、化合物収率 5%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物
触媒
HCID 31374Dimethylacetamide溶媒

反応条件

温度
80 °C

実験手順

A stirred mixture of 3-bromo-7-trifluoromethylimidazo[1,2-c]pyrimidine (100 mg, 0.375 mmol), dried potassium phosphate (0.159 g, 0.750 mmol) and 2′-fluoro-5′-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)biphenyl-2-carbonitrile (0.2424 g, 0.750 mmol) in anhydrous N,N-dimethylacetamide (2 ml) was degassed by evacuation and refilling with nitrogen three times. Tetrakis(triphenylphosphine)palladium(0) (22 mg, 0.019 mmol) was then added and the mixture was degassed with two more evacuation-refilling cycles before heating at 80° C. under nitrogen for 3 h. The mixture was partitioned between ethyl acetate (250 ml) and brine (250 ml), and the aqueous layer was extracted further with ethyl acetate (250 ml). The combined organic extracts were dried (Na2SO4) and evaporated in vacuo. The residue was purified by flash chromatography (silica gel, 40% EtOAc/isohexane), then recrystallisation (EtOAc) to give 6.8 mg (5%) of the title compound: 1H NMR (400 MHz, CDCl3) δ 7.46 (1H, t, J 8.6 Hz), 7.56 (1H, td, J 7.7, 1.3 Hz), 7.60 (1H, m), 7.65-7.74 (3H, m), 7.85 (1H, dd, J 7.8, 1.6 Hz), 7.89 (1H, s), 7.99 (1H, s), 9.37 (1H, s); MS (ES+) m/z 383 [M+H]+.

後処理

  1. customwas degassed by evacuation and refilling with nitrogen three times
  2. customthe mixture was degassed with two more evacuation-refilling cycles
  3. customThe mixture was partitioned between ethyl acetate (250 ml) and brine (250 ml)
  4. extractionthe aqueous layer was extracted further with ethyl acetate (250 ml)
  5. dry with materialThe combined organic extracts were dried (Na2SO4)
  6. customevaporated in vacuo
  7. customThe residue was purified by flash chromatography (silica gel, 40% EtOAc/isohexane)
  8. customrecrystallisation (EtOAc)

出典と根拠

ORDレコード
ord-a22f2195a4934042ac355cb13a3dfcba
出典データセット
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06914065B2

反応ノート

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