반응식
[NH2:1][C:2]1[S:6][C:5]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[C:4]([CH3:12])[C:3]=1[C:13]([O:15]CC)=O.[S:18]1[CH:22]=[CH:21][C:20]([CH2:23][C:24]#[N:25])=[CH:19]1.Cl.O1CCOCC1.N>>[CH3:12][C:4]1[C:3]2[C:13](=[O:15])[NH:25][C:24]([CH2:23][C:20]3[CH:21]=[CH:22][S:18][CH:19]=3)=[N:1][C:2]=2[S:6][C:5]=1[C:7]([O:9][CH2:10][CH3:11])=[O:8]참가 물질
5
실험 절차
515 Milligrams of diethyl 5-amino-3-methylthiophene-2,4-dicarboxylate and 296 mg of 3-thiopheneacetonitrile were added to 8 mL of 4N hydrogen chloride-dioxane solution and stirred for 10 hours. Thereafter the liquid reaction mixture was poured on ice, and its pH was adjusted to 8-9 with 25% aqueous ammonia. Whereupon precipitated crystals were recovered by filtration and washed first with water, and then with hexane. The crude crystals were recrystallized from a liquid mixture of N,N-dimethylformamide and cyclohexane, to provide 397 mg of the title compound.
후처리
- customThereafter the liquid reaction mixture
- additionwas poured on ice, and its pH
- customWhereupon precipitated crystals
- filtrationwere recovered by filtration
- washwashed first with water
- customThe crude crystals were recrystallized from a liquid mixture of N,N-dimethylformamide and cyclohexane
출처 및 근거
- ORD 기록
- ord-c9af8f1317034c27b6e3a3a0c5a95503
- 출처 데이터셋
- uspto-grants-2013_02
- 특허 번호
- US08377944B2
연결된 노트
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