Water → 1-(4-Chlorobenzoyl)-3-[4-(5,6,7,8-tetrahydro-2-naphthyl-)2-thiazolyl]thiourea
反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][CH:3]=1.[S-:11][C:12]#[N:13].[NH4+].[NH2:15][C:16]1[S:17][CH:18]=[C:19]([C:21]2[CH:30]=[CH:29][C:28]3[CH2:27][CH2:26][CH2:25][CH2:24][C:23]=3[CH:22]=2)[N:20]=1.O>CC(C)=O>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH:13][C:12]([NH:15][C:16]2[S:17][CH:18]=[C:19]([C:21]3[CH:30]=[CH:29][C:28]4[CH2:27][CH2:26][CH2:25][CH2:24][C:23]=4[CH:22]=3)[N:20]=2)=[S:11])=[O:7])=[CH:4][CH:3]=1参加物
実験手順
4-Chlorobenzoyl chloride (911 mg) was added to a solution of ammonium thiocyanate (460 mg) in acetone (20 ml), and the solution mixture was heated over a water bath for 1 minute and stirred at room temperature for 1 hour. A solution of 2-amino-4-(5,6,7,8-tetrahydro-2-naphthyl)thiazole (1.0 g) in acetone (10 ml) was added to the solution, followed by stirring at room temperature for 16 hours. The reaction mixture was poured into water, and the crystals which separated out were recovered by filtration and washed with water and hexane, successively. Recrystallization from dichloromethane-ethanol produced 1-(4-chlorobenzoyl)-3-[4-(5,6,7,8-tetrahydro-2-naphthyl-)2-thiazolyl]thiourea (Yield of 1.08 g, 58.1%) %) in the form of colorless needles. m.p. 193° to 194° C.
後処理
- temperaturethe solution mixture was heated over a water bath for 1 minute
- stirringby stirring at room temperature for 16 hours
- customthe crystals which separated out
- filtrationwere recovered by filtration
- washwashed with water and hexane
- customRecrystallization from dichloromethane-ethanol
出典と根拠
- ORDレコード
- ord-27e5b20268c8499987e7eef6e059e188
- 出典データセット
- uspto-grants-1994_04
- 特許番号
- US05302608
反応ノート
読み込み中…