反应详情

温度

120 °C

An eggplant flask was charged with 2-methoxymethyl-1-(tetrahydropyran-4-yl)-5-trifluoromethylbenzimidazole (see Working Example 6-1) (0.102 g, 0.32 mmol), 2-aminobenzenethiol (0.041 g, 0.33 mmol) and polyphosphoric acid (approx. 2 g), and this was heated to 120° C. and stirred for 48 hours. After being allowed to cool, ice was added and concentrated aqueous ammonia (28%) was added to the liquid to give approx. pH 9. Chloroform extraction, drying over anhydrous magnesium sulfate, and the solvent being distilled off gave a crude product (0.21 g), which was purified by silica gel column chromatography (MeOH/CHCl3=1/20) to yield the title compound (0.010 g, 8.1% yield) as a pale yellow powder.

1. temperatureto cool
2. additionice was added
3. customto give approx. pH 9
4. extractionChloroform extraction
5. dry with materialdrying over anhydrous magnesium sulfate
6. distillationthe solvent being distilled off
7. customgave a crude product (0.21 g), which
8. customwas purified by silica gel column chromatography (MeOH/CHCl3=1/20)