反应详情

温度

25 °C

To a stirred solution of 5-mercapto-1-methyltetrazole sodium salt hydrate (1.1 g., 0.008 mole) in aqueous ethanol (15 ml), a solution of cis-4-thiocyano-3-buten-2-one (Compound 28) in ethanol was added dropwise over 5 minutes. A solid suspension was observed forming over the next 2 hours which was stirred at 25° C. for 18 hours. The volatiles were removed in vacuo and the residue was extracted into ethyl acetate and washed thoroughly with water. After drying (MgSO4), the solution was concentrated. The solid residue was purified via column chromatography on silica gel using hexanes/ethyl acetate (3:2) as eluant to yield 1.1 g of a white solid, mp 112°-114° C. IR (nujol) uc=o 1660 cm-1.

1. customA solid suspension was observed forming over the next 2 hours which
2. customThe volatiles were removed in vacuo
3. extractionthe residue was extracted into ethyl acetate
4. washwashed thoroughly with water
5. dry with materialAfter drying (MgSO4)
6. concentrationthe solution was concentrated
7. customThe solid residue was purified via column chromatography on silica gel