Sodium Bicarbonate → 9-bromo-2-carboxymethyloxy-5-(3-pyridylmethyl)-4H-pyrido [3,2,1-jk]carbazole-4-one

HRID 1530985ノート

反応式

HRID 1530985 の反応式
[Br:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6]4=[C:7]([C:24](=[O:34])[C:25]([CH2:27][C:28]5[CH:29]=[N:30][CH:31]=[CH:32][CH:33]=5)=[CH:26][N:5]4[C:4]=2[CH:3]=1)[CH:8]=[C:9]([O:15][CH2:16][C:17]([O:19]C(C)(C)C)=[O:18])[CH:10]=3.C(=O)([O-])O.[Na+]>C(O)(=O)C.Br>[Br:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6]4=[C:7]([C:24](=[O:34])[C:25]([CH2:27][C:28]5[CH:29]=[N:30][CH:31]=[CH:32][CH:33]=5)=[CH:26][N:5]4[C:4]=2[CH:3]=1)[CH:8]=[C:9]([O:15][CH2:16][C:17]([OH:19])=[O:18])[CH:10]=3

参加物

5

反応物 2

HCID 516892Sodium BicarbonateHCID 193648749-bromo-2-t-butoxycarbonylmethyloxy-5-(3-pyridylmethyl)-4H-pyrido [3,2,1-jk]carbazole-4-one

生成物 1

HCID 193648899-bromo-2-carboxymethyloxy-5-(3-pyridylmethyl)-4H-pyrido [3,2,1-jk]carbazole-4-one収率 79%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 260Hydrogen Bromide溶媒

実験手順

9-bromo-2-t-butoxycarbonylmethyloxy-5-(3-pyridylmethyl)-4H-pyrido [3,2,1-jk]carbazole-4-one (57 mg) produced in Example 103 was dissolved in acetic acid (0.5 ml) and 48% HBr (0.5 ml), and the solution was stirred at 60° C. for 1 hour and allowed to cool. Saturated aqueous solution of sodium hydrogencarbonate was added to pH 7, and the crystals precipitated were recovered by filtration, washed with water, ethanol and ether in succession, and recovered by filtration to obtain the title compound (40 mg, 79%).

後処理

  1. temperatureto cool
  2. customthe crystals precipitated
  3. filtrationwere recovered by filtration
  4. washwashed with water, ethanol and ether in succession
  5. filtrationrecovered by filtration

出典と根拠

ORDレコード
ord-6bee209921954d41bd39196d5e53b354
出典データセット
uspto-grants-2001_03
特許番号
US06197768B1

反応ノート

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