HRID1169019

反应详情

EQUATION

反应方程式

HRID 1169019 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a one-liter, round bottom 3-necked flask, fitted with a mechanical stirrer, thermometer and dropping funnel, was added 118 g of glycerin carbonate (I) (1.0 moles) and 200 ml. of dry tetrahydofuran (THF). After addition of 1.0 g dimethylcyclohexylamine (DMCHA), the resulting solution was stirred under nitrogen at ambient temperature. Then, 87 g (1.0 equiv.) of Rubinate® 80/20 (Huntsman Corp.) toluenediisocyanate (TDI) (II) was then added dropwise while controlling the exothermic reaction so that the temperature did not exceed 60° C. After the addition of compound II was complete the reaction product was maintained at 50° C. for one hour. The resulting product was primarily a solution of III in THF, a light yellow mobile liquid. The reaction is shown diagrammatically below.

WORKUP

后处理

  1. customTo a one-liter, round bottom 3-necked flask, fitted with a mechanical stirrer
  2. customthe exothermic reaction so that the temperature
  3. customdid not exceed 60° C
  4. temperaturewas maintained at 50° C. for one hour