反応式
[Na][Na].[C:3]([C:5]1[C:9](=[C:10]([C:13]#[N:14])[C:11]#[N:12])[NH:8][C:7](=[O:15])[C:6]=1O)#[N:4].[CH2:17]([CH:19]([CH2:31][CH2:32][CH2:33][CH3:34])[CH2:20][N:21]([CH2:28][CH2:29][CH3:30])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[CH3:18].P(Cl)(Cl)(Cl)=O>CC(C)=O.O.CN(C)C=O>[CH2:17]([CH:19]([CH2:31][CH2:32][CH2:33][CH3:34])[CH2:20][N:21]([C:22]1[CH:23]=[CH:24][C:25]([C:6]2[C:7](=[O:15])[NH:8][C:9](=[C:10]([C:13]#[N:14])[C:11]#[N:12])[C:5]=2[C:3]#[N:4])=[CH:26][CH:27]=1)[CH2:28][CH2:29][CH3:30])[CH3:18]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 3
反応条件
- 温度
- -10 °C
実験手順
A stirred mixture of disodium salt of 4-cyano-5-dicyanomethylidene-3-hydroxy-2-oxo-2,5-dihydropyrrole (29.9 parts) and dry N,N-dimethylformamide (150 parts) was cooled to -10° C. and N-(2-ethylhexyl)-N-propylaniline containing 30% acetic anhydride (63 parts) was added followed by the dropwise addition of phosphorous oxychloride (34 parts) maintaining the temperature at less than -5°C. The mixture was allowed to warmup to room temperature and stirred for 20 hours. The reaction mixture was poured into a stirred mixture of ice and water (200 parts) and acetone (200 parts) and then stirred for 0.5 hours. The solid was filtered off, washed with hot water and dried under vacuum to give 3-(4-(N-(2-ethylhexyl)-N-propylamino)phenyl)-4-cyano-5-dicyanomethylidene-2-oxo-2,5-dihydropyrrole (48.5 parts, 90%).
後処理
- temperaturemaintaining the temperature at less than -5°C
- customto warmup to room temperature
- stirringstirred for 0.5 hours
- filtrationThe solid was filtered off
- washwashed with hot water
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-b707bb1bdd8a46fa9be047c3f4b62f7f
- 出典データセット
- uspto-grants-1997_08
- 特許番号
- US05660598
関連ノート
読み込み中…