反応 #68739

反応方程式

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

methyl acrylate

acetic acid

→

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

溶媒

反応条件

後処理

1. 1
   その他A 100 ml 3-neck flask was fitted with an overhead stirrer
2. 2
   抽出extracted with aqueous sodium hydroxide
3. 3
   洗浄washed three times with water
4. 4
   その他Solvent was removed by rotary evaporation
5. 5
   その他Some polymer precipitated
6. 6
   その他was removed
7. 7
   その他Solvent was removed by rotary evaporation
8. 8
   ろ過filtered
9. 9
   その他Solvent was removed by rotary evaporation
10. 10
    その他Remaining volatiles were removed by vacuum distillation (29″, 196° C.)
11. 11
    その他to yield a viscous, dark yellow liquid

実験手順

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.

出典