Hydrogen Peroxide → 5-(2-Methylpropyl)-8-[3-(trifluoromethyl)phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one
反応式
S=[C:2]1[N:12]2[C:13]3[N:8]([C:9]([C:14]4[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=4)=[CH:10][CH2:11]2)[N:7]=[CH:6][C:5]=3[C:4](=[O:24])[NH:3]1.[OH-].[Na+].OO.[CH2:29](N)[CH:30]([CH3:32])[CH3:31]>CN(C)C=O>[CH3:29][CH:30]([CH3:32])[CH2:31][C:2]1[N:12]2[C:13]3[N:8]([C:9]([C:14]4[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=4)=[CH:10][CH2:11]2)[N:7]=[CH:6][C:5]=3[C:4](=[O:24])[N:3]=1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 0 °C
実験手順
To a solution of 500 mg of 4,5-dihydro-5-thioxo-8-[3-(trifluoromethyl)phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one (prepared as described in Example 8) in 10.0 ml of N,N-dimethylformamide was added 1.5 ml of 1N sodium hydroxide. The reaction mixture was cooled to 0° C. in an ice bath, then 0.5 ml of 30% hydrogen peroxide was added to the mixture dropwise. The reaction mixture was stirred at 0° C. for 30 minutes, then 1.0 ml of isobutylamine was added in one portion and the mixture was allowed to warm to room temperature, then was stirred for 2 hours. The solid was collected by filtration and washed with water, then ether to give 223 mg of the product of the example as a white solid, m.p. 266°-268° C. Following the procedure of Example 14 and reacting, 4,5-dihydro-5-thioxo-8-[3-(trifluoromethyl)phenyl]3H ,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one with the appropriate primary aliphatic amine or cyclic secondary amine, the products of Examples 15-27 were obtained as set forth in Table III.
後処理
- temperatureto warm to room temperature
- stirringwas stirred for 2 hours
- filtrationThe solid was collected by filtration
- washwashed with water
出典と根拠
- ORDレコード
- ord-f71a7546a89e403c9615866a626c22af
- 出典データセット
- uspto-grants-1990_04
- 特許番号
- US04916137
反応ノート
読み込み中…