反応式
[C:1]([OH:9])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1.[Cl:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([Cl:17])[C:12]=1[NH:18][C:19]1[NH:20][CH2:21][CH2:22][N:23]=1>O1CCCC1>[C:1]([N:23]1[CH2:22][CH2:21][N:20]=[C:19]1[NH:18][C:12]1[C:13]([Cl:17])=[CH:14][CH:15]=[CH:16][C:11]=1[Cl:10])(=[O:9])[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1参加物
実験手順
5.5 g (44.7 millimoles) of nicotinic acid are dissolved in 800 ml of absolute tetrahydrofuran, 7.3 g (45 millimoles) of N,N'-carbonyldiimidazole are added and the mixture is stirred for 45 minutes at room temperature. A solution of 10.3 g (44.7 millimoles) of 2-(2',6'-dichlorophenylamino)-2-imidazoline in 200 ml of absolute tetrahydrofuran is then added dropwise, with continued stirring, and the mixture is left to stand overnight at room temperature. Thereafter, the reaction solution is freed from solvent on a rotary evaporator, 200 ml of an 0.5% strength sodium bicarbonate solution are added to the residue, and the product which precipitates is filtered off and washed with water. After drying, the crude product is recrystallized from isopropanol. 7.2 g of 1-nicotinoyl-2-(2',6'-dichlorophenylamino)-2-imidazoline, melting point 173°-174° C., are obtained.
後処理
- waitthe mixture is left
- waitto stand overnight at room temperature
- customThereafter, the reaction solution is freed from solvent on a rotary evaporator, 200 ml of an 0.5% strength sodium bicarbonate solution
- additionare added to the residue
- customthe product which precipitates
- filtrationis filtered off
- washwashed with water
- customAfter drying
- customthe crude product is recrystallized from isopropanol
出典と根拠
- ORDレコード
- ord-77f6547408474775a0609fc09c348a00
- 出典データセット
- uspto-grants-1983_06
- 特許番号
- US04389403
関連ノート
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