HRID371370

反应详情

EQUATION

反应方程式

HRID 371370 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Approximately 360 g of the 1,2-mixed pentadecanedioloctadecanediol (obtained from Viking Chemical Co. as Vikol 158 containing about 28% 1,2-pentadecanediol, about 28% 1,2-hexadecanediol, about 28% 1,2-heptadecanediol and about 16% 1,2-octadecanediol) were charged to a glass reactor equipped with heater, agitator, Dean-Stark tube with condenser and provision for blanketing the vapor space with nitrogen. The contents were heated to 70° C. to liquify and 55 g of dimethyl hydrogen phosphite were slowly added. The reaction mixture was heated to 110° C. and held for 2 hours, held at 120° C. for 1 hour, and held at 130° C. for 1 hour. During this reaction period, methanol distilled over and condensed into the trap. The crude product was vacuum stripped at 150° C. to remove volatile materials. 379 g of finished additive were produced. The product was an amber fluid which became waxy on cooling.

WORKUP

后处理

  1. customequipped with heater, agitator, Dean-Stark tube with condenser
  2. temperatureThe reaction mixture was heated to 110° C.
  3. waitheld at 120° C. for 1 hour
  4. waitheld at 130° C. for 1 hour
  5. distillationdistilled over and
  6. customcondensed into the trap
  7. customstripped at 150° C.
  8. customto remove volatile materials
  9. custom379 g of finished additive were produced
  10. temperatureon cooling