反应详情

温度

80 °C

4 N hydrochloric acid (50 cc) is added to the sodium salt of 1-(2,2-dimethyl-1,3-dioxan-5-yl)-5-mercaptotetrazole (as obtained in accordance with Example 7) (22 g) in water (100 cc) and the mixture is heated for 30 minutes at 80° C. 4 N sodium hydroxide solution (25 cc) is added and the mixture is concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa). The residue is taken up in boiling acetonitrile (2×100 cc), an insoluble material is filtered off, the acetonitrile is evaporated off under reduced pressure (20 mm Hg; 2.7 kPa) and the residue is taken up in ethyl ether (100 cc). 1-(1,3-Dihydroxyprop-2-yl)-5-mercaptotetrazole (11 g), melting at 138° C., is isolated by filtration.

1. concentrationthe mixture is concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa)
2. filtrationan insoluble material is filtered off
3. customthe acetonitrile is evaporated off under reduced pressure (20 mm Hg; 2.7 kPa)