HRID2234922
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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 hours. The mixture was concentrated in vacuo to give a yellow solid which was filtered and washed with methanol. The filtrate was concentrated and the process repeated. On the final wash the filtrate was purified by SPE (Si, 20 g) cartridge eluting with 1:1; EtOAc:cyclohexane. The combined solids were dried under vacuum to afford the title compound (2.42 g, 64%); m/z 283.3 [MH+]
WORKUP
后处理
- waitleft
- concentrationThe mixture was concentrated in vacuo
- customto give a yellow solid which
- filtrationwas filtered
- washwashed with methanol
- concentrationThe filtrate was concentrated
- washOn the final wash the filtrate
- customwas purified by SPE (Si, 20 g) cartridge
- washeluting with 1:1
- customThe combined solids were dried under vacuum