反应详情

Following the procedure 2(A) described in this application, to a 100 ml round bottom flask equipped with a stir bar and reflux condenser topped with a nitrogen inlet was added 5 g (0.03 mol) tris(hydroxymethyl)nitromethane, 2.86 g (0.04 mol) ethylvinyl ether, 50 ml acetonitrile and 5 drops concentrated HCl. The reaction was heated to 35°-40° C. for 4 hours. After cooling to room temperature the volatiles were removed to give the product, 2-methyl-5-hydroxymethyl-5-nitro-1,3-dioxane, in 86% yield. 1H NMR in CD3OD confirmed the structure.

1. customdescribed in this application, to a 100 ml round bottom flask
2. customequipped with a stir bar
3. temperaturereflux condenser
4. customtopped with a nitrogen inlet
5. temperatureThe reaction was heated to 35°-40° C. for 4 hours
6. customwere removed