反应详情

A mixture of p-methoxybenzyl α-thioformamidodiethylphosphonoacetate (188 mg., 0.5 mmole), powdered potassium carbonate (1.52 mg., 1.1 mmole) and chloro-2-propanone (44μl., 0.55 mmole) in acetone (2.5 ml.) is stirred at room temperature and under a nitrogen atmosphere. After 22 hours stirring, the mixture is filtered and the salts washed with acetone. The combined filtrate and washings are evaporated in vacuo to a dark residue which is shaken with csrbon tetrachloride (3 × 2 ml.). The combined extracts are washed with water (2 × 2 ml.) and saturated brine (2 ml.), dried over magnesium sulfate and evaporated in vacuo to give p-methoxybenzyl 5-methyl-6H-1,3-thiazine-4-carboxylate (116 mg.) as an orange oil.

1. stirringAfter 22 hours stirring
2. filtrationthe mixture is filtered
3. washthe salts washed with acetone
4. customThe combined filtrate and washings are evaporated in vacuo to a dark residue which
5. stirringis shaken with csrbon tetrachloride (3 × 2 ml.)
6. washThe combined extracts are washed with water (2 × 2 ml.) and saturated brine (2 ml.)
7. dry with materialdried over magnesium sulfate
8. customevaporated in vacuo