HRID1097639

反应详情

EQUATION

反应方程式

HRID 1097639 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-butyl-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (3.34 g, 13.4 mmol) in anhydrous DMF (19 ml) was added NCS (1.97 g, 14.8 mmol) and left to stir at rt under nitrogen for 22 h. The mixture was concentrated in vacuo to give a yellow solid which was filtered and washed with MeOH to provide a first crop. The filtrate was concentrated to a solid and washed with MeOH to provide a second crop and repeated a further two occasions to provide the title compound. On the final wash the filtrate was further purified by SPE (Si, 20 g) cartridge eluting with EtOAc:cyclohexane (1:1). The combined solids were dried under vacuum to afford the title compound (2.42 g, 64%).

WORKUP

后处理

  1. waitleft
  2. concentrationThe mixture was concentrated in vacuo
  3. customto give a yellow solid which
  4. filtrationwas filtered
  5. washwashed with MeOH
  6. customto provide a first crop
  7. concentrationThe filtrate was concentrated to a solid
  8. washwashed with MeOH
  9. customto provide a second crop