반응 #4790

반응 방정식

2-isocyanatoethyl methacrylate

diethanolamine

methylhydroquinone

→

2-[N',N'-Bis(2-hydroxyethyl)ureido]ethyl Methacrylate

용매

toluene

반응 조건

후처리

1. 1
   workup.ADDITIONwas dropped slowly in the flask
2. 2
   온도was maintained at 20° to 25° C. with an ice-bath
3. 3
   workup.STIRRINGThe resulting viscous solution was stirred for an additional 60 minutes at 20° C.
4. 4
   기타no NCO absorption in the IR spectrum
5. 5
   workup.ADDITIONAdditional inhibitor was added (to a total of 250 ppm) and the diol

실험 절차

A one liter flask, under a N2 blanket, was charged with 105 gm of diethanolamine (1 mole) and 20 mg of methylhydroquinone. One molar of 2-isocyanatoethyl methacrylate (IEM) containing 2 ml of DBTDL (2% solution in toluene) was dropped slowly in the flask with moderate stirring over a period of 105 minutes, while the temperature was maintained at 20° to 25° C. with an ice-bath. The resulting viscous solution was stirred for an additional 60 minutes at 20° C. and then discharged. The product showed no NCO absorption in the IR spectrum and the NMR spectrum was consistent with the proposed structure. Gas chromatography also indicated the purity of the product to be greater than 95%. Additional inhibitor was added (to a total of 250 ppm) and the diol was stored in a freezer.

출처