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Triethylamine → 3-(Imidazo[1,2-b]pyridazin-6-ylethynyl)aniline

HRID 589912
ノート
印刷プレビュー

反応式

HRID 589912 の反応式
O[C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[CH:9][N:10]=2)[N:7]=1.C(N(CC)CC)C.C1C=CC(N(S(C(F)(F)F)(=O)=O)S(C(F)(F)F)(=O)=O)=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:58]([C:60]1[CH:61]=[C:62]([CH:64]=[CH:65][CH:66]=1)[NH2:63])#[CH:59]>CN(C=O)C.C(OCC)(=O)C.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[Cu]I>[N:10]1[CH:9]=[CH:8][N:6]2[C:5]=1[CH:4]=[CH:3][C:2]([C:59]#[C:58][C:60]1[CH:61]=[C:62]([CH:64]=[CH:65][CH:66]=1)[NH2:63])=[N:7]2
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 104682Benzenamine, 3-ethynyl-HCID 142176Phenyl triflimideHCID 178515753HCID 178515753、化合物

生成物 1

HCID 1186384153-(Imidazo[1,2-b]pyridazin-6-ylethynyl)aniline

試薬・触媒・溶媒 4

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 178418476HCID 178418476、化合物触媒
HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a stirring mixture of 6-hydroxyimidazo[1,2-b]pyridazine (2.06 g, 15.259 mmol, 1 eq) in anhydrous DMF (20 mL) under nitrogen atmosphere was added triethylamine (8.51 mL, 4 eq) and N-phenyl-bis(trifluoromethanesulfonimide) (5.386 g, 1 eq). After the reaction was stirred at room temperature for 18 hours, to the reaction was added triphenylphosphine (100 mg, 0.025 eq), bis(triphenylphosphine)palladium(II) dichloride (1.07 g, 0.1 eq), copper(I) iodide (581 mg, 0.2 eq), and 3-ethynylaniline (2.394 mL, 1.5 eq) under nitrogen atmosphere. The resulting reaction mixture was heated at 60° C. for two hours. The reaction was then cooled to room temperature, diluted with ethyl acetate, washed sequentially with aqueous ammonium chloride, saturated aqueous sodium bicarbonate, brine, and lastly dried with anhydrous sodium sulfate. The upper solution was decanted, concentrated, the residue mixture was subject to a gradient column chromatography (from DCM to MeOH-DCM 1:25). The product fractions were collected, concentrated, and the residue was triturated with EtOAc-Hex (˜1:5) to give 3-(imidazo[1,2-b]pyridazin-6-ylethynyl)aniline as a fluffy slightly yellow solid upon filtration in amount of 2.384 g (67%).

後処理

  1. customThe resulting reaction mixture
  2. temperaturewas heated at 60° C. for two hours
  3. temperatureThe reaction was then cooled to room temperature
  4. washwashed sequentially with aqueous ammonium chloride, saturated aqueous sodium bicarbonate, brine
  5. dry with materiallastly dried with anhydrous sodium sulfate
  6. customThe upper solution was decanted
  7. concentrationconcentrated
  8. customThe product fractions were collected
  9. concentrationconcentrated
  10. customthe residue was triturated with EtOAc-Hex (˜1:5)

出典と根拠

ORDレコード
ord-56c80f63f9c34e66ba65b4845b762e31
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09233968B1

反応ノート

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