HRID862903

反应详情

EQUATION

反应方程式

HRID 862903 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5-(5-chlorosulphonyl-2-hydroxyphenyl)-1-methyl-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]pyrimidin-7-one (0.235 g, 0.0006 mol) and N-methylpiperazine (0.5 ml, 0.0045 mol) in ethanol (40 ml) was stirred at room temperature for 18 hours. The solution was evaporated under vacuum and the residue partitioned between ethyl acetate (40 ml) and water (40 ml). The fine precipitate was filtered off, washed with water then ethyl acetate, and crystallised from ethyl acetate/DMF to give the title compound as an off-white powder (0.260 g, 49%), m.p. 283°-284° C. Found: C,53.53; H,5.89; N,18.40. C20H26N6O4S requires C,53.80; H,5.87; N,18.82%.

WORKUP

后处理

  1. customThe solution was evaporated under vacuum
  2. customthe residue partitioned between ethyl acetate (40 ml) and water (40 ml)
  3. filtrationThe fine precipitate was filtered off
  4. washwashed with water
  5. customethyl acetate, and crystallised from ethyl acetate/DMF