反应详情

To a magnetically stirred stined suspension of 10/5 g (40 mmol) of 1-(2',6'-diethylphenyl)-3-ethylamidinourea in 10 ml of CH3CN is added 9.52 g (80 mmol) of N,N-dimethylformamide dimethylacetal and another 20 ml of CH3CN. The reaction mixture is heated to reflux at which point all of the solid dissolves. The solution is refluxed for one hour, allowed to cool to ambient temperature and then concentrated in vacuo to yield an off-white solid which is taken up in CHCl3, washed with H2O) (2×50 ml) and saturated aqueous brine (2×25 ml). All aqueous wash layers are combined and back-extracted with CHCl3, (2×25 ml). All organic layers are combined, dried (Na2SO2), filtered and the filtrate concentrated in vacuo to yield a yellow oil. The oil is taken up in MeOH and acidified with HCl/MeOH then concentrated in vacuo.

1. temperatureThe reaction mixture is heated
2. temperatureto reflux at which point all of the solid
3. dissolutiondissolves
4. temperatureThe solution is refluxed for one hour
5. concentrationconcentrated in vacuo
6. customto yield an off-white solid which
7. washwashed with H2O) (2×50 ml) and saturated aqueous brine (2×25 ml)
8. extractionback-extracted with CHCl3, (2×25 ml)
9. dry with materialdried (Na2SO2)
10. filtrationfiltered
11. concentrationthe filtrate concentrated in vacuo
12. customto yield a yellow oil
13. concentrationthen concentrated in vacuo