反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder reflux for 9 hours
- customclear solution is formed
- customThe product is precipitated from acetonitrile
- filtrationfiltered under suction
- washwashed with acetone
- customdried under a slight vacuum
- customat 210° C.
- customis obtained in a yield of 93%
- filtrationthe precipitated urea was filtered off