Ethanol → 10-bromo-2-carboxymethyloxy-5-methyl-4H-pyrido[3,2,1-jk]carbazole-4-one

HRID 1530965노트

반응식

HRID 1530965 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]3[CH:24]=[C:23]([CH3:25])[C:22](=[O:26])[C:8]4[CH:9]=[C:10]([O:15][CH2:16][C:17]([O:19]CC)=[O:18])[CH:11]=[C:12]([C:13]=2[CH:14]=1)[C:7]3=4.C(O)C.[OH-].[Na+]>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]3[CH:24]=[C:23]([CH3:25])[C:22](=[O:26])[C:8]4[CH:9]=[C:10]([O:15][CH2:16][C:17]([OH:19])=[O:18])[CH:11]=[C:12]([C:13]=2[CH:14]=1)[C:7]3=4

참가 물질

5

반응물 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 1936490610-bromo-2-ethoxycarbonylmethyloxy-5-methyl-4H-pyrido[3,2,1-jk]carbazole-4-one

생성물 1

HCID 1936493110-bromo-2-carboxymethyloxy-5-methyl-4H-pyrido[3,2,1-jk]carbazole-4-one수율 91.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

10-bromo-2-ethoxycarbonylmethyloxy-5-methyl-4H-pyrido [3,2,1-jk]carbazole-4-one (200 mg) obtained in Example 52 was suspended in a mixed solution of ethanol (10 ml) and methylene chloride (10 ml), and IN aqueous solution of sodium hydroxide (1 ml) was added to the suspension. The mixture was stirred at room temperature for 90 minutes, and the solvent was evaporated under reduced pressure. To the residue was added water and 1N hydrochloric acid to pH 1, and the crystals precipitated were recovered by filtration to obtain the title compound (170 mg, 91%).

후처리

  1. customthe solvent was evaporated under reduced pressure
  2. additionTo the residue was added water and 1N hydrochloric acid to pH 1
  3. customthe crystals precipitated
  4. filtrationwere recovered by filtration

출처 및 근거

ORD 기록
ord-277381a9af9c4168bac20d74beee42a5
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06197768B1

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