反応 #55488

反応方程式

isobutyraldehyde

urea

sodium hydroxide

sulfuric acid

→

Urea isobutyraldehyde

溶媒

water

xylene

water

反応条件

後処理

1. 1
   温度heated to the boil, in a stirred flask
2. 2
   その他equipped with a condenser
3. 3
   その他The resulting water (158 parts) is removed via the water separator
4. 4
   その他During the condensation reaction
5. 5
   その他rises to 123°-125° C
6. 6
   その他is removed at the boil until the temperature
7. 7
   その他reaches 132°-135° C
8. 8
   workup.ADDITION60 Parts of 30% strength sodium methylate solution in methanol are then added to the contents of the flask, which
9. 9
   workup.STIRRINGare stirred for 1 hour at the boil (112°-115° C.)
10. 10
    洗浄washed with 1,000 parts of water at 80° C
11. 11
    その他After separating off the wash water
12. 12
    workup.DISTILLATIONthe solvent is distilled from the xylene phase under reduced pressure (20-25 mm Hg)
13. 13
    その他being 175° C.

実験手順

864 Parts of isobutyraldehyde, 800 parts of xylene and 240 parts of urea are mixed, and heated to the boil, in a stirred flask equipped with a condenser, water separator, thermometer and dropping funnel. 50 Parts of 75% strength sulfuric acid are added dropwise in the course of about 10 minutes and the mixture is then stirred for 5 hours at the boil. The resulting water (158 parts) is removed via the water separator. During the condensation reaction, the temperature rises to 123°-125° C. The mixture is then cooled to 80° C. and neutralized with about 50 parts of 50% strength sodium hydroxide solution, and further water is removed at the boil until the temperature reaches 132°-135° C. 60 Parts of 30% strength sodium methylate solution in methanol are then added to the contents of the flask, which are stirred for 1 hour at the boil (112°-115° C.). The mixture is then cooled to 60° C., neutralized with 75% strength sulfuric acid and washed with 1,000 parts of water at 80° C. After separating off the wash water, the solvent is distilled from the xylene phase under reduced pressure (20-25 mm Hg), the temperature in the flask being 175° C.

出典