2-Bromopropiophenone → 2-Amino-4-phenyl-5-methylthiazole
반응식
Br[CH:2]([CH3:11])[C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=O.[NH2:12][C:13]([NH2:15])=[S:14]>CCO>[CH3:11][C:2]1[S:14][C:13]([NH2:15])=[N:12][C:3]=1[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1참가 물질
4
실험 절차
A mixture of 2-bromo-1-phenylpropan-1-one (3.00 g, 19.5 mmol) and thiourea (1.56 g, 20.5 mmol) in 95% EtOH (30 mL) was heated at reflux for 60 min. The solution was concentrated and mixed with water (100 mL) and saturated aqueous Na2CO3 (5.0 mL). The resultant precipitate was filtered and recrystallized in toluene. The solids were filtered and dried under vacuum to give 5-methyl-4-phenylthiazol-2-amine (4.07 g) as yellow solids in 77% yield: 1H NMR (500 MHz, DMSO-d6) δ 8.85 (s, 2 H), 7.54-7.49 (m, 5 H), 2.28 (s, 3 H).
후처리
- temperaturewas heated
- temperatureat reflux for 60 min
- concentrationThe solution was concentrated
- additionmixed with water (100 mL) and saturated aqueous Na2CO3 (5.0 mL)
- filtrationThe resultant precipitate was filtered
- customrecrystallized in toluene
- filtrationThe solids were filtered
- customdried under vacuum
출처 및 근거
- ORD 기록
- ord-2122b380754b49ad9e43237b9a4f6d0c
- 출처 데이터셋
- uspto-grants-2015_04
- 특허 번호
- US08999983B2
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