HRID235566

反应详情

EQUATION

反应方程式

HRID 235566 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A methyllithium solution in ether (1.4M, 40 ml) was added to a solution of 1.0 g of N-[(4,6-dimethoxypyrimidin-2-yl)aminocarbonyl]-2-carboxybenzenesulfonamide in 50 ml of dry tetrahydrofuran at room temperature. The resulting yellow slurry was stirred for 4 hours and the dilute hydrochloric acid was added. The mixture was then extracted with methylene chloride. The organic extracts were washed, dried, and evaporated in vacuo to dryness. The crude product was purified by preparative TLC, eluted with ethyl acetate/hexane (1:1), m.p. 126°-128° C.

WORKUP

后处理

  1. extractionThe mixture was then extracted with methylene chloride
  2. washThe organic extracts were washed
  3. customdried
  4. customevaporated in vacuo to dryness
  5. customThe crude product was purified by preparative TLC
  6. washeluted with ethyl acetate/hexane (1:1), m.p. 126°-128° C.