HRID1980391

反应详情

EQUATION

反应方程式

HRID 1980391 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

1420 g of 1-(p-tert.butylphenyl)-2-formyl-1-propene, prepared as described in paragraph (e), are mixed together with 6 g of 5% palladium/carbon and 6.8 g of soda in 20 ml of water at 70°-75° C. in a stirring autoclave. The autoclave is charged with hydrogen (8 atmospheres) and heated to 110° C. About 230 liters of hydrogen are absorbed after 12 hours. The crude 3-(p-tert.butyl-phenyl)-2-methyl-propionaldehyde is treated with ether, washed neutral with water and dried over sodium sulphate. After removing the ether, the product is fractionally distilled in vacuo. After separating a first running and a last running, there are obtained 1275 g of 3-(p-tert.butyl-phenyl)-2-methyl-propionaldehyde in 95% purity (about 88% of theory). Boiling point: 150°-152° C./15 mmHg; nD20 =1.5050.

WORKUP

后处理

  1. customAbout 230 liters of hydrogen are absorbed after 12 hours
  2. additionThe crude 3-(p-tert.butyl-phenyl)-2-methyl-propionaldehyde is treated with ether
  3. washwashed neutral with water
  4. dry with materialdried over sodium sulphate
  5. customAfter removing the ether
  6. distillationthe product is fractionally distilled in vacuo
  7. customAfter separating a first running