反应详情

In tetrahydrofuran (100 ml), 4-chloro-2-methoxybenzamide (9.40 g, 50.6 mmol) prepared in the Step 7-1-1 and Lawesson's reagent (10.2 g, 25.3 mmol) were suspended, and the suspension was heated under reflux for 2 hours. After the suspension was allowed to cool, a saturated sodium bicarbonate solution was added to the suspension to stop the reaction. Then the reaction mixture was subjected to extraction with ethyl acetate, and the extract was dried over anhydrous magnesium sulfate and then concentrated. The concentrate was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:1) to give the title compound (6.63 g, 65%) as a yellow powder.

1. temperaturethe suspension was heated
2. temperatureunder reflux for 2 hours
3. temperatureto cool
4. customthe reaction
5. extractionThen the reaction mixture was subjected to extraction with ethyl acetate
6. dry with materialthe extract was dried over anhydrous magnesium sulfate
7. concentrationconcentrated
8. customThe concentrate was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:1)