反应详情

To a solution of 0.30 g of 2-amino-5-[(4-acetyl-3-hydroxy-2-propylbenzyl)thio]-1,3,4-thiadiazole obtained in Example 5 in 6.5 ml of pyridine was dropwise added 0.20 g of ethyloxalyl chloride at -30° C. The mixture was stirred at room temperature for 30 minutes. Water was added to the reaction mixture followed by extraction with ethyl acetate After the extract was dried over anhydrous magnesium sulfate, the solvent was distilled off. The residue was subjected to silica gel column chromatography. Elution with a solvent mixture of chloroform-ethyl acetate (8:1) gave 0.15 g of ethyl [5-[(4-acetyl-3-hydroxy-2-propylbenzyl)thio]- 1,3,4-thiadiazol-2-yl]oxamate.

1. customat -30° C
2. extractionfollowed by extraction with ethyl acetate After the extract
3. dry with materialwas dried over anhydrous magnesium sulfate
4. distillationthe solvent was distilled off
5. washElution
6. additionwith a solvent mixture of chloroform-ethyl acetate (8:1)