反応式
[Br:1][C:2]1[C:23]([O:24]C)=[CH:22][C:5]2[C:6]([CH3:21])([CH3:20])[C:7]3[NH:8][C:9]4[C:14]([C:15]=3[C:16](=[O:17])[C:4]=2[CH:3]=1)=[CH:13][CH:12]=[C:11]([C:18]#[N:19])[CH:10]=4.C[O-].[Na+].C(S)CCCCCCCCCCC.Cl>CN1C(=O)CCC1>[Br:1][C:2]1[C:23]([OH:24])=[CH:22][C:5]2[C:6]([CH3:21])([CH3:20])[C:7]3[NH:8][C:9]4[C:14]([C:15]=3[C:16](=[O:17])[C:4]=2[CH:3]=1)=[CH:13][CH:12]=[C:11]([C:18]#[N:19])[CH:10]=4参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 160 °C
実験手順
9-Bromo-8-methoxy-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (Compound E3-1-1, 1.0 g, 2.53 mmol) was dissolved in NMP (10 mL), added with NaOMe (683 mg, 5 eq.) and 1-dodecanethiol (3.0 mL, 5 eq.), and stirred at 160° C. for 1 hr. The reaction solution was added to 0.5 N aqueous solution of hydrochloric acid, and then extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were added with MeOH, and the solid remaining after dissolution was filtered to obtain the title compound (yellow powder, 1.88 g, 65%).
後処理
- extractionextracted with ethyl acetate
- washThe organic layer was washed with saturated brine
- dry with materialdried over sodium sulfate
- customThe drying agent was removed by filtration
- customthe residues obtained
- concentrationafter concentration under reduced pressure
- additionwere added with MeOH
- dissolutionafter dissolution
- filtrationwas filtered
出典と根拠
- ORDレコード
- ord-411dd9c632f3437ab2c91d13e9f98145
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09440922B2
関連ノート
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