反应详情

2-(3-Chloropropan-1-yl)oxybenzonitrile (503 mg) was added, at room temperature, to an acetonitrile solution (20 ml) of N-(piperidin-4-yl)-5-thia-1,8b-diazaacenaphthylene-4-carboxamide dihydrochloride (800 mg), 1,8-diazabicyclo[5.4.0]-7-undecene (662 mg), triethylamine (1.09 g) and sodium iodide (285 mg). The mixture was heated under reflux for 7.5 hours under nitrogen atmosphere. The reaction mixture was concentrated under reduced pressure. To the concentrate was added water, which was subjected to extraction with chloroform. The extract solution was washed with a saturated aqueous saline solution, which was dried over anhydrous magnesium sulfate, followed by concentration under reduced pressure. The concentrate was purified by means of a silica gel column chromatography (ethyl acetate/methanol=2/1) to afford the object compound (816 mg, 83%) as a reddish purple oily product.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 7.5 hours under nitrogen atmosphere
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. additionTo the concentrate was added water, which
5. extractionwas subjected to extraction with chloroform
6. washThe extract solution was washed with a saturated aqueous saline solution, which
7. dry with materialwas dried over anhydrous magnesium sulfate
8. concentrationfollowed by concentration under reduced pressure
9. customThe concentrate was purified by means of a silica gel column chromatography (ethyl acetate/methanol=2/1)