HRID1944025

反应详情

EQUATION

反应方程式

HRID 1944025 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
77 °C

PROCEDURE

实验过程

To EtOH (27.8 L), triethyl orthoformate (9.26 L, 55.6 mol) and diethyl 4-oxopimelate (5.93 L, 27.8 mol) was added p-toluenesulfonic acid monohydrate (0.053 kg, 0.278 mol), and the reaction mixture was heated to 77.0° C. with stirring for 20 h. Heating was discontinued, and ethanol was removed by distillation under vacuum, starting with the batch at 63° C. The remaining orange ketal solution was dissolved in toluene (32 L) and transferred to a 100-L extractor that had been charged with 2% NaHCO3 (24 L), with stirring.

WORKUP

后处理

  1. temperatureHeating
  2. customethanol was removed by distillation under vacuum
  3. customstarting with the batch at 63° C
  4. dissolutionThe remaining orange ketal solution was dissolved in toluene (32 L)
  5. additionhad been charged with 2% NaHCO3 (24 L)
  6. stirringwith stirring