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Potassium Carbonate → 10-bromo-2-(3-pyridylmethyloxy)-4H-pyrido[3,2,1-jk]carbazole-4-one

HRID 850769
ノート
印刷プレビュー

反応式

HRID 850769 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]3[CH:18]=[CH:17][C:16](=[O:19])[C:8]4[CH:9]=[C:10]([OH:15])[CH:11]=[C:12]([C:13]=2[CH:14]=1)[C:7]3=4.C(=O)([O-])[O-].[K+].[K+].Cl.[N:27]1[CH:32]=[CH:31][CH:30]=[C:29]([CH2:33]Cl)[CH:28]=1>CS(C)=O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]3[CH:18]=[CH:17][C:16](=[O:19])[C:8]4[CH:9]=[C:10]([O:15][CH2:33][C:29]5[CH:28]=[N:27][CH:32]=[CH:31][CH:30]=5)[CH:11]=[C:12]([C:13]=2[CH:14]=1)[C:7]3=4
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 233943-(Chloromethyl)pyridine hydrochlorideHCID 2125288410-bromo-2-hydroxy-4H-pyrido[3,2,1-jk]carbazole-4-one

生成物 1

HCID 1936491610-bromo-2-(3-pyridylmethyloxy)-4H-pyrido[3,2,1-jk]carbazole-4-one収率 52%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

10-bromo-2-hydroxy-4H-pyrido[3,2,1-jk]carbazole-4-one (300 mg) obtained in Example 59 was suspended in dimethyl sulfoxide (20 ml), and potassium carbonate (400 mg) was added to the suspension. The mixture was stirred at room temperature for 30 minutes and 3-picolylchloride hydrochloride (180 mg) was added and the mixture was stirred at room temperature for 12 hours. The reaction mixture was poured into ice water (100 ml), and the precipitated crystals were recovered by filtration. The resulting crude crystals were washed with methanol and ether in succession, and recovered by filtration to obtain the title compound (200 mg, 52%).

後処理

  1. stirringthe mixture was stirred at room temperature for 12 hours
  2. filtrationthe precipitated crystals were recovered by filtration
  3. washThe resulting crude crystals were washed with methanol and ether in succession
  4. filtrationrecovered by filtration

出典と根拠

ORDレコード
ord-454e999fde2441a08bfebbf003c3f8b1
出典データセット
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06018046

反応ノート

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