反应详情

To a stirring solution of p-methoxybenzyl α-thioformamido-diethylphosphonoacetate (114 mg., 0.3 mmole) in acetone (1.5 ml.) is added powdered potassium carbonate (124 mg., 0.9 mmole). The resulting mixture is stirred for 5 minutes at room temperature and under a nitrogen atmosphere, then treated with a solution of 1-acetoxy-3-chloro-2-propanone (48 mg., 0.32 mmole) in acetone (0.5 ml.). After having been stirred for 3 hours at room temperature, the mixture is filtered to remove the salts which are washed with acetone. The combined filtrate and washings are evaporated in vacuo to a dark oil. The residue is dissolved in carbon tetrachloride (6 ml.), washed with aqueous phosphate (1 ml. of 1M dipotassium phosphate + 2 ml. water) and water (2 × 3 ml.), dried over magnesium sulfate, and evaporated in vacuo to give crude p-methoxybenzyl 5-acetoxymethyl-6H-1,3-thiazine-4-carboxylate (106 mg.) as an organic oil.

1. stirringAfter having been stirred for 3 hours at room temperature
2. filtrationthe mixture is filtered
3. customto remove the salts which
4. washare washed with acetone
5. customThe combined filtrate and washings are evaporated in vacuo to a dark oil
6. dissolutionThe residue is dissolved in carbon tetrachloride (6 ml.)
7. washwashed with aqueous phosphate (1 ml. of 1M dipotassium phosphate + 2 ml. water) and water (2 × 3 ml.)
8. dry with materialdried over magnesium sulfate
9. customevaporated in vacuo