HRID2396795

反应详情

EQUATION

反应方程式

HRID 2396795 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of tetrahydropyrrolo[1,2-b]-1,2,5-thiadiazol-3(2H)-one 1,1-dioxide (5.0 g, 28.4 mmol) suspended in 150 ml of toluene was added phenylthiomethyl chloride (6.76 g, 42.6 mmol) and tetrabutylammonium bromide (0.91 g) . The resulting mixture was refluxed for 6 hours, cooled, filtered, and the filtrate was concentrated in vacuo. The residue was purified by flash column chromatography (25-30% ethyl acetate in hexane) to afford 5.58 g (66%) of 2-phenylthiomethyl-tetrahydropyrrolo[1,2-b]-1,2,5-thiadiazol-3(2H)_-one 1,1-dioxide (Formula VI: R1 =H; R2 and R3 together=--(CH2)3 --) as a solid, m.p. 90.5°-91.5° C.

WORKUP

后处理

  1. temperatureThe resulting mixture was refluxed for 6 hours
  2. temperaturecooled
  3. filtrationfiltered
  4. concentrationthe filtrate was concentrated in vacuo
  5. customThe residue was purified by flash column chromatography (25-30% ethyl acetate in hexane)