반응 #497538
ord-742fe5ff1016404b89c8dad0a1fdc0d1
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시약
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후처리
- 1온도The mixture was heated
- 2온도to reflux where it
- 3온도was maintained for 48 h
- 4온도The reaction was then heated
- 5온도to reflux for a further 15 h
- 6온도It was then cooled to rt
- 7여과filtered
- 8기타The collected solid was dried
실험 절차
To a solution of 1-(4-bromo-benzyl)-6-methyl-1,3-dihydro-benzoimidazol-2-ylideneamine (0.14 g, 0.44 mmol) in 2-butanone (5 ml) at rt was added 1-(3-bromo-propoxy)-4-fluoro-benzene (0.15 g, 0.66 mmol). The reaction was stirred for 10 min and then additional 2-butanone (5 ml) was introduced. The mixture was heated to reflux where it was maintained for 48 h. After this time, the reaction was cooled to rt and additional 1-(3-bromo-propoxy)-4-fluoro-benzene (0.05, 0.22 mmol) was added. The reaction was then heated to reflux for a further 15 h. It was then cooled to rt and filtered. The collected solid was dried to provide 3-(4-bromo-benzyl)-1-[3-(4-fluoro-phenoxy)-propyl]-5-methyl-1,3-dihydrobenzoimidazol-2-ylideneamine, hydrobromide salt (0.04 g, 16%). HPLC-MS 468, 470 [M+1]+.