Thiourea → HCID 58442508、化合物
反応式
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]=1参加物
4
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-61139ffa1fe6408a979590ad28013401
- 出典データセット
- uspto-grants-2015_02
- 特許番号
- US08946268B2
反応ノート
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