HRID2186440

反应详情

EQUATION

反应方程式

HRID 2186440 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.025 mol of hydroxypropyl cellulose (DS 0.9) and 0.0125 mol of triethylamine are refluxed for 30 minutes in 150 g of dioxane. 0.05 mol of stearoyl isocyanate is then added dropwise and the suspension is stirred under reflux for 9 hours. In the course of this a highly viscous. clear solution is formed. The product is precipitated from acetonitrile, filtered under suction, washed with acetone and dried under a slight vacuum. A white product, which forms a melt of low viscosity at 210° C. and contains bis-stearoyl urea, is obtained in a yield of 93%. (FT-IR: C═O stretching vibration, urethane 1720 cm−1; C═O stretching vibration, urea 1615 cm−1; N—H deformation vibration, urea 1575 cm−1). To control the IR spectra, the bis-stearoyl urea was prepared directly by reacting 0.05 mol of stearoyl isocyanate with 0.1 mol of water in 100 g of dioxane, the precipitated urea was filtered off and the FT-IR spectrum was recorded: (FT-IR: C═O stretching vibration, urea 1615 cm−1; N—H deformation vibration, urea 1575 cm−1).

WORKUP

后处理

  1. temperatureunder reflux for 9 hours
  2. customclear solution is formed
  3. customThe product is precipitated from acetonitrile
  4. filtrationfiltered under suction
  5. washwashed with acetone
  6. customdried under a slight vacuum
  7. customat 210° C.
  8. customis obtained in a yield of 93%
  9. filtrationthe precipitated urea was filtered off