반응 #70584

반응 방정식

2-bromo-1-(2-phenylpyrimidin-5-yl)ethanone

thiobenzamide

→

title compound

수율 46.0%

2-phenyl-4-(2-phenylpyrimidin-5-yl)thiazole

수율 46.0%

용매

ethanol

반응 조건

후처리

1. 1
   온도was heated
2. 2
   workup.WAITto near boiling for several minutes
3. 3
   기타A white solid precipitated within minutes
4. 4
   여과The precipitate was collected by vacuum filtration
5. 5
   세척Light ethanol rinse
6. 6
   기타suction, and drying under high vacuum at room temperature

실험 절차

A mixture consisting of 2-bromo-1-(2-phenylpyrimidin-5-yl)ethanone (Example 14, Step B, 50 mg, 0.18 mmol), thiobenzamide (TCl America, 25 mg, 0.18 mmol) and absolute ethanol (4 mL) in a capped scintillation vial was heated to near boiling for several minutes and was subsequently allowed to cool to room temperature. A white solid precipitated within minutes. The precipitate was collected by vacuum filtration. Light ethanol rinse, suction, and drying under high vacuum at room temperature afforded the title compound (26 mg, 46% yield) as an off-white solid; melting point 214.4-216.1° C.; 1H-NMR (400 MHz; DMSO-d6) δ 9.54 (s, 2H), 8.54 (s, 1H), 8.47 (m, 2H), 8.08 (m, 2H), 7.62-7.54 (m, 6H); LC/MS (ESI+) m/z 316.1, (ESI−) m/z 337.2 (M−1+Na+); H-PGDS FPBA IC50: >20 μM.

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