ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

3-Fluoroaniline → HCID 59409476、化合物

HRID 659954
ノート
印刷プレビュー

反応式

HRID 659954 の反応式
Cl[C:2]1[CH:7]=[C:6]([C:8]2[N:16]([CH2:17][CH2:18][F:19])[C:15]3[C:10](=[N:11][CH:12]=[CH:13][CH:14]=3)[C:9]=2[C:20]2[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=2)[CH:5]=[CH:4][N:3]=1.[F:27][C:28]1[CH:29]=[C:30]([NH2:34])[CH:31]=[CH:32][CH:33]=1.C1(C2C=CC=CC=2)C=CC=CC=1P(C1CCCCC1)C1CCCCC1.CC(C)([O-])C.[Na+].[Cl-].[NH4+]>C1(C)C=CC=CC=1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[F:19][CH2:18][CH2:17][N:16]1[C:15]2[C:10](=[N:11][CH:12]=[CH:13][CH:14]=2)[C:9]([C:20]2[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=2)=[C:8]1[C:6]1[CH:5]=[CH:4][N:3]=[C:2]([NH:34][C:30]2[CH:31]=[CH:32][CH:33]=[C:28]([F:27])[CH:29]=2)[CH:7]=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

8

反応物 5

HCID 97423-FluoroanilineHCID 25517Ammonium ChlorideHCID 27342162-(Dicyclohexylphosphino)biphenylHCID 23676156Sodium t-butoxideHCID 86643499HCID 86643499、化合物

生成物 1

HCID 59409476HCID 59409476、化合物収率 38.2%

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 1140Toluene溶媒

反応条件

温度
180 °C

実験手順

In a 5 mL microwave vessel (Biotage) are weighted together 185 mg (0.5 mmole) of 2-(2-Chloro-pyridin-4-yl)-1-(2-fluoro-ethyl)-3-(4-fluoro-phenyl)-1H-pyrrolo[3,2-b]pyridine, 67 mg (0.6 mmoles) of 3-fluorophenyl amine, 2 mg of palladium acetate, 7 mg of biphenylyl dicyclohexylphosphine and 67 mg (0.7 mmole) of sodium t-butoxide in 2.5 mL of toluene. The reaction mixture is then heated at 180° C. for 10 min. under microwave conditions. The reaction mixture is poured into ammonium chloride solution and extracted with ethyl acetate. The organic phase is washed with water and dried over magnesium sulfate. After concentration the solid residue is purified by chromatography on silica gel (ethyl acetate/hexane 1/1) to give 85 mg of {4-[1-(2-Fluoro-ethyl)-3-(4-fluoro-phenyl)-1H-pyrrolo[3,2-b]pyridin-2-yl]-pyridin-2-yl}-(3-fluoro-phenyl)-amine as white solid.

後処理

  1. customIn a 5 mL microwave vessel (Biotage) are weighted together
  2. extractionextracted with ethyl acetate
  3. washThe organic phase is washed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationAfter concentration the solid residue
  6. customis purified by chromatography on silica gel (ethyl acetate/hexane 1/1)

出典と根拠

ORDレコード
ord-f3390600c1fc42f08045e461c41a568f
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08084395B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート