反应 #1880995

反应方程式

8-(4-Hydroxy-bicyclo[2.2.2]oct-1-yl)-6-(1-hydroxymethyl-propylamino)-3-propyl-3,7-dihydro-purin-2-one

→

titled compound

收率 47.7%

7-Ethyl-2-(4-hydroxy-bicyclo[2.2.2]oct-1-yl)4-propyl-1,4,6,7-tetrahydro-1,3,4,5a,8-pentaaza-as-indacen-5-one

收率 47.7%

溶剂

SOCl2

反应条件

后处理

1. 1
   温度under reflux for 20 min
2. 2
   浓缩concentrated
3. 3
   其他The residue was quenched with saturated aq NaHCO3
4. 4
   萃取extracted with CHCl3
5. 5
   干燥The combined organic layers were dried (Na2SO4)
6. 6
   浓缩concentrated under reduced pressure
7. 7
   其他Purification by preparative HPLC

实验过程

8-(4-Hydroxy-bicyclo[2.2.2]oct-1-yl)-6-(1-hydroxymethyl-propylamino)-3-propyl-3,7-dihydro-purin-2-one (110 mg) was dissolved in 3 mL of SOCl2 and stirred under reflux for 20 min. It was then cooled to rt and concentrated. The residue was quenched with saturated aq NaHCO3 and extracted with CHCl3. The combined organic layers were dried (Na2SO4) and concentrated under reduced pressure. Purification by preparative HPLC afforded 50 mg of the titled compound as the TFA salt.

来源