反应 #52247

反应方程式

Hydroxy ethylmaleimide

isophorone diisocyanate

→

Isophorone Bisurethane Bisethylmaleimide

溶剂

acetone

反应条件

后处理

1. 1
   其他purged with nitrogen
2. 2
   workup.ADDITIONOne drop of dibutyl tin dilaurate was added to the solution
3. 3
   workup.STIRRINGto stir overnight
4. 4
   其他a white precipitate was obtained
5. 5
   其他after solvent removal m.p. 105-112° C. (40.5 g, 100%)

实验过程

Hydroxy ethylmaleimide (10 g, 0.141 mol) was dissolved in acetone and purged with nitrogen while stirring in an ice bath. One drop of dibutyl tin dilaurate was added to the solution. The isophorone diisocyanate (30.5 g, 0.141 mol) was added dropwise over 2-3 hours. The solution was allowed to stir overnight and a white precipitate was obtained after solvent removal m.p. 105-112° C. (40.5 g, 100%). 1H-NMR (D6-DMSO, δ, ppm): 3.63-3.58 (2H, —NCH2—), 4.08-4.03 (2H, —CH2O—, t), 7.03 (2H, —CH═CH—, s). 13C-NMR (D6-DMSO, δ, ppm): 134.5 (2C, —CH═CH—), 154.9 (2C, NHC═O), (170.7 (2C, —NC═O).

来源