반응 #68739

반응 방정식

N,N,N′-tricyclohexyl-para-phenylenediamine

methyl acrylate

acetic acid

→

N,N,N′-tricyclohexyl-N′-methoxypropionyl-para-phenylenediamine

용매

반응 조건

후처리

1. 1
   기타A 100 ml 3-neck flask was fitted with an overhead stirrer
2. 2
   추출extracted with aqueous sodium hydroxide
3. 3
   세척washed three times with water
4. 4
   기타Solvent was removed by rotary evaporation
5. 5
   기타Some polymer precipitated
6. 6
   기타was removed
7. 7
   기타Solvent was removed by rotary evaporation
8. 8
   여과filtered
9. 9
   기타Solvent was removed by rotary evaporation
10. 10
    기타Remaining volatiles were removed by vacuum distillation (29″, 196° C.)
11. 11
    기타to yield a viscous, dark yellow liquid

실험 절차

A 100 ml 3-neck flask was fitted with an overhead stirrer, a thermocouple and a nitrogen inlet. The flask was charged with N,N,N′-tricyclohexyl-para-phenylenediamine (27.1 g), methyl acrylate (150 ml) and glacial acetic acid (10 ml). The reaction was stirred at 82° C. until complete. The reaction mass was taken up in xylenes, extracted with aqueous sodium hydroxide and washed three times with water. Solvent was removed by rotary evaporation. The reaction mass was taken up in hexanes. Some polymer precipitated and was removed. Solvent was removed by rotary evaporation. The product was taken up in xylenes and filtered. Solvent was removed by rotary evaporation. Remaining volatiles were removed by vacuum distillation (29″, 196° C.) to yield a viscous, dark yellow liquid.

출처