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Potassium Carbonate → 10-bromo-5-methyl-2-(3-pyridylmethyloxy)-4H-pyrido[3,2,1-jk]carbazole-4-one

HRID 850759
ノート
印刷プレビュー

反応式

HRID 850759 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]3[CH:18]=[C:17]([CH3:19])[C:16](=[O:20])[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:28]1[CH:33]=[CH:32][CH:31]=[C:30]([CH2:34]Cl)[CH:29]=1>CS(C)=O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]3[CH:18]=[C:17]([CH3:19])[C:16](=[O:20])[C:8]4[CH:9]=[C:10]([O:15][CH2:34][C:30]5[CH:29]=[N:28][CH:33]=[CH:32][CH:31]=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 2125284210-bromo-2-hydroxy-5-methyl-4H-pyrido [3,2,1-jk]carbazole-4-one

生成物 1

HCID 1936487210-bromo-5-methyl-2-(3-pyridylmethyloxy)-4H-pyrido[3,2,1-jk]carbazole-4-one収率 60.4%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

10-bromo-2-hydroxy-5-methyl-4H-pyrido[3,2,1-jk]carbazole-4-one (350 mg) obtained in Example 49 was suspended in dimethyl sulfoxide (14 ml), and potassium carbonate (440 mg) was added to the suspension. The mixture was stirred at room temperature for 30 minutes and 3-picolylchloride hydrochloride (190 mg) was added to the mixture. The mixture was stirred at room temperature for 12 hours, and the reaction mixture was poured into ice water (500 ml). The crystals precipitated 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 (270 mg, 60%).

後処理

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

出典と根拠

ORDレコード
ord-888378f2bc034ff3997406cbc802754b
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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