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Ammonia → HCID 17864574、化合物

HRID 1592944
ノート
印刷プレビュー

反応式

HRID 1592944 の反応式
Cl.Br[C:3]1[CH:12]=[C:11]2[C:6]([C:7]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([F:20])=[C:16]([Cl:21])[CH:15]=3)=[N:8][CH:9]=[N:10]2)=[CH:5][C:4]=1[N+:22]([O-:24])=[O:23].[CH3:25][C:26]([N:30]1[CH2:35][CH2:34][N:33]([CH3:36])[CH2:32][CH2:31]1)([CH3:29])[C:27]#[CH:28].C(N(CC)CC)C.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N>CS(C)=O.[Cu](Cl)Cl.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(OCC)(=O)C>[Cl:21][C:16]1[CH:15]=[C:14]([NH:13][C:7]2[C:6]3[C:11](=[CH:12][C:3]([C:28]#[C:27][C:26]([CH3:29])([N:30]4[CH2:31][CH2:32][N:33]([CH3:36])[CH2:34][CH2:35]4)[CH3:25])=[C:4]([N+:22]([O-:24])=[O:23])[CH:5]=3)[N:10]=[CH:9][N:8]=2)[CH:19]=[CH:18][C:17]=1[F:20]
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

10

反応物 5

HCID 222AmmoniaHCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 17864580(7-Bromo-6-nitro-4-quinazolinyl)-(3-chloro-4-fluorophenyl)amine hydrochlorideHCID 22354399HCID 22354399、化合物

生成物 1

HCID 17864574HCID 17864574、化合物収率 50%

試薬・触媒・溶媒

4
HCID 24014Cupric Chloride触媒HCID 167845palladium(II) acetate触媒HCID 679Dimethyl Sulfoxide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

A solution of (7-bromo-6-nitro-4-quinazolinyl)-(3-chloro-4-fluorophenyl)amine hydrochloride (42.0 g, 96.8 mmol), 1-(1,1-dimethyl-2-propynyl)-4-methylpiperazine (4a) (19.3 g, 116 mmol) and triethylamine (47.2 mL, 339 mmol) in DMSO (400 mL) was subjected 3 times to the step of degassing under reduced pressure and then displacement with nitrogen. Copper iodide (I) (460.8 mg, 2.4 mmol), triphenylphosphine (2.53 g, 9.6 mmol) and palladium(II) acetate (543 mg, 2.4 mmol) were added. The mixture was stirred at 80° C. for 9 hrs and allowed to cool to room temperature. The mixture was poured into ethyl acetate (750 mL) and 1% aqueous ammonia solution (1.5 L), and Celite (50 g) was added, which was followed by stirring. Insoluble material was filtered off and the organic layer was washed with brine (500 mL×2) and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and ethyl acetate-methanol mixed solvent (10:1, 130 mL) was added to the residue. The mixture was stirred and the precipitate was collected by filtration. The filtered product was suspension-washed with acetonitrile (100 mL) and dried to give a nitro compound 3a (23.3 g, 48.3 mmol, 50%).

後処理

  1. customof degassing under reduced pressure
  2. temperatureto cool to room temperature
  3. additionwas added
  4. stirringby stirring
  5. filtrationInsoluble material was filtered off
  6. washthe organic layer was washed with brine (500 mL×2)
  7. dry with materialdried over anhydrous sodium sulfate
  8. customThe solvent was evaporated under reduced pressure and ethyl acetate-methanol mixed solvent (10:1, 130 mL)
  9. additionwas added to the residue
  10. stirringThe mixture was stirred
  11. filtrationthe precipitate was collected by filtration
  12. washThe filtered product was suspension-washed with acetonitrile (100 mL)
  13. customdried

出典と根拠

ORDレコード
ord-90e2fce3d6b3406b9668e6e7981db074
出典データセット
uspto-grants-2007_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07294629B2

反応ノート

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