HRID248860

反应详情

EQUATION

反应方程式

HRID 248860 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
220 °C

PROCEDURE

实验过程

3,000 g of 3-(4-tert.-butylphenyl)-2-methylprop-2-enal III and 2,000 g of vinyl isobutyl ether IV are introduced into a 10 l stirred autoclave, and 5 g of hydroquinone are added to the reaction mixture for stabilization. The autoclave is closed and then flushed with nitrogen, after which it is heated to 220° C., maintained under these conditions for 18 hours and then let down and opened. The reaction mixture (4,855 g) consists of about 39.6% of the desired product V. When the reaction mixture is worked up by fractionation in a laboratory column containing 10 sieve trays, a total of 1,379 g of the compound V of boiling point 135°-146° C. under 2 mbar are obtained from the 1,923 g shown to be present in the crude mixture by gas chromatographic analysis. This corresponds to a yield of 23%, based on the starting material III employed. 1,745 g of III, which contains some product V, are recovered. The last-mentioned amounts are reused for the reaction with vinyl isobutyl ether.

WORKUP

后处理

  1. additionare added to the reaction mixture for stabilization
  2. customThe autoclave is closed
  3. customflushed with nitrogen
  4. temperaturemaintained under these conditions for 18 hours
  5. additioncontaining 10 sieve trays