HRID1899877

反应详情

EQUATION

反应方程式

HRID 1899877 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5-(benzenesulfanyl)-thiazolidine-2,4-dione, [(III), Example 6, 10.0 g, 41.8 mmol] in methanol (105 mL) was added to a mechanically stirred suspension of oxone (51.4 g, 83.6 mmol) in water (210 mL) at 0° C. The suspension was immediately warmed to room temperature. After 3.5 h, the reaction was diluted with water (1.5 L) and the solid was filtered. The solid was washed with water and dried in vacuo to provide the title compound as a white solid (8.31 g, 73%): mp 130°-133° C.: NMR (CDCL3): δ 8.07 (s, 1H, NH), 7.98 (d, J=7.2 Hz, 2H, ArH) 7.78 (t, J=7.5 Hz, 1H, ArH), 7.67 (t, J=8.1Hz, 2H, ArH), 5.44 (s, 1H CH); MS(EI): 225 (MI, 24%), 182 (18%), 153 (12%), 110 (100%). By the procedure described in Example 15, the compounds of formula (V), Examples 16-18, were prepared from the appropriate 5-(arylsulfanyl)-thiazolidine-2,4-dione of formula (III).

WORKUP

后处理

  1. filtrationthe solid was filtered
  2. washThe solid was washed with water
  3. customdried in vacuo