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A mixture of 3.3 g of 2-nitroacetophenone and 2.94 g of 2-(methylthio)-5,6-dihydro-4H-1,3-thiazine was heated to 115° and 100 milligrams of zinc chloride was added. Heating and stirring was continued at 115°-120° for 2.5 hours. After cooling, the mixture was filtered (with the aid of ethyl acetate) through a short column of florosil to give an amber oil. The oil was chromatographed on silica gel using dry-column technique and a 1:1:2 mixture of tetrahydrofuran/ethyl acetate/hexane for development to give 1 as a salmon-colored solid, m.p.: 137°-140°.

1. temperaturewas heated to 115°
2. temperatureHeating
3. temperatureAfter cooling
4. filtrationthe mixture was filtered (with the aid of ethyl acetate) through a short column of florosil
5. customto give an amber oil
6. customThe oil was chromatographed on silica gel using dry-column technique
7. additiona 1:1:2 mixture of tetrahydrofuran/ethyl acetate/hexane for development