HRID27211

反应详情

EQUATION

反应方程式

HRID 27211 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 800 parts of 2-methylpentanal, 800 parts of xylene and 120 parts of urea is heated to the boil in a stirred apparatus of the type described in Example 1, and 50 parts of 75% strength sulfuric acid are added dropwise. The mixture is then stirred at the boil and the water formed (84 parts) is removed via the water separator. The condensation is complete after about 3 hours. The reaction mixture is neutralized with 50% strength sodium hydroxide solution and stirred for a further hour at the boil, whilst removing water. 60 Parts of 30% strength sodium methylate solution in methanol are then added to the contents of the flask and the mixture is again stirred for 1 hour at the boil. It is then cooled to 60° C., neutralized to pH 7 with 75% strength sulfuric acid and washed with twice 1,000 parts of water. After removing the wash water, the xylene solution is evaporated under reduced pressure (20-25 mm Hg) until the temperature in the flask reaches 175° C.

WORKUP

后处理

  1. temperatureis heated to the boil in a stirred apparatus of the type
  2. additionare added dropwise
  3. customis removed via the water separator
  4. stirringstirred for a further hour at the boil
  5. customwhilst removing water
  6. addition60 Parts of 30% strength sodium methylate solution in methanol are then added to the contents of the flask
  7. stirringthe mixture is again stirred for 1 hour at the boil
  8. washwashed with twice 1,000 parts of water
  9. customAfter removing the wash water
  10. customthe xylene solution is evaporated under reduced pressure (20-25 mm Hg) until the temperature in the flask
  11. customreaches 175° C.