Thiourea → HCID 58442508, 화합물
반응식
Br[CH2:2][C:3]([C:5]1[C:10]([CH3:11])=[CH:9][C:8]([Cl:12])=[CH:7][C:6]=1[CH3:13])=O.[NH2:14][C:15]([NH2:17])=[S:16]>CCO>[Cl:12][C:8]1[CH:9]=[C:10]([CH3:11])[C:5]([C:3]2[N:14]=[C:15]([NH2:17])[S:16][CH:2]=2)=[C:6]([CH3:13])[CH:7]=1참가 물질
4
실험 절차
A mixture of 2-bromo-1-(4-chloro-2,6-dimethylphenyl)ethanone (6.54 g, 25.0 mmol) and thiourea (1.90 g, 25.0 mmol) in 95% EtOH (35.7 mL) was heated at reflux for 60 min. The solution was concentrated and added with water (50 mL) followed by saturated aqueous Na2CO3 (4.0 mL). The resultant precipitate was filtered and recrystallized in toluene (30 mL). The solids were filtered and dried under vacuum to give 4-(4-chloro-2,6-dimethylphenyl)thiazol-2-amine (4.30 g) as white solids in 72% yield: 1H NMR (500 MHz, DMSO-d6) δ 7.16 (s, 2 H), 6.43 (s, 1 H), 2.10 (s, 6 H).
후처리
- temperaturewas heated
- temperatureat reflux for 60 min
- concentrationThe solution was concentrated
- additionadded with water (50 mL)
- filtrationThe resultant precipitate was filtered
- customrecrystallized in toluene (30 mL)
- filtrationThe solids were filtered
- customdried under vacuum
출처 및 근거
- ORD 기록
- ord-61139ffa1fe6408a979590ad28013401
- 출처 데이터셋
- uspto-grants-2015_02
- 특허 번호
- US08946268B2
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