Water → 1-(4-Chlorobenzoyl)-3-[4-(5,6,7,8-tetrahydro-2-naphthyl-)2-thiazolyl]thiourea
반응식
[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]=1참가 물질
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-27e5b20268c8499987e7eef6e059e188
- 출처 데이터셋
- uspto-grants-1994_04
- 특허 번호
- US05302608
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