HRID1736318
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a mixture of 4-propyl-1,2,5-thiadiazolidin-3-one 1,1-dioxide (5.1 g, 28.65 mmol) suspended in 210 ml of toluene was added tetrabutylammonium bromide (0.92 g, 2.86 mmol) and phenylthiomethyl chloride (4.93 g, 2.86 mmol) and the resulting mixture was refluxed for 18 hours. The mixture was cooled, filtered, and the filtrate was concentrated in vacuo. The residue was purified by silica gel flash column chromatography (20% ethyl acetate in hexane) to afford 5.39 g (63%) of 2-phenylthiomethyl-4-propyl-1,2,5-thiadiazolidin-3-one 1,1-dioxide (Formula VI: R1 =H; R2 =propyl; R3 =H).
WORKUP
后处理
- temperaturethe resulting mixture was refluxed for 18 hours
- temperatureThe mixture was cooled
- filtrationfiltered
- concentrationthe filtrate was concentrated in vacuo
- customThe residue was purified by silica gel flash column chromatography (20% ethyl acetate in hexane)