HRID648069

反应详情

EQUATION

反应方程式

HRID 648069 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

196.13 g (1 mole) of methyl N-(4-nitrophenyl)-carbamate, 108.14 g (1 mole) of 3-aminomethyl-pyridine and 106.7 g (0.5 mole) of N,N-dimethyl-n-dodecylamine are dissolved in 3 liters of xylene. The reaction mixture is refluxed, and the spures of water present are removed from the mixture together with the alcohol formed in a Dean-Stark trap. The end-product starts to separate from the mixture within 15-20 minutes from the beginning of boiling. The mixture is boiled for 4 hours, thereafter the suspension is filtered at about 100° to 110° C. The filter cake is washed twice with 100 ml of hot xylene, each, and with a small amount of acetone, and then dried in vacuo. 218.6 g (80.3%) of N-(4-nitrophenyl)-N'-(3-pyridylmethyl)-urea are obtained; m.p.: 221°-223° C.

WORKUP

后处理

  1. temperatureThe reaction mixture is refluxed
  2. customthe spures of water present are removed from the mixture together with the alcohol
  3. customformed in a Dean-Stark trap
  4. customto separate from the mixture within 15-20 minutes from the beginning of boiling
  5. filtrationthe suspension is filtered at about 100° to 110° C
  6. washThe filter cake is washed twice with 100 ml of hot xylene
  7. dry with materialeach, and with a small amount of acetone, and then dried in vacuo