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Acetoacetanilide: Aniline in Ether with Diketene Added Slowly (Gleason, Standard Oil Development, US 2,174,239)
Diketene and aniline join into acetoacetanilide, the coupling component of Hansa yellow, but neat they react so violently that the product is poor. Gleason tamed the reaction by diluting both in ether and adding the diketene slowly; the anilide simply crystallises out.
Result: crystals of acetoacetanilide.
Source: Gleason, US 2,174,239 (Standard Oil Development, 1939). Not given: yield. Picture drawn by Youblob.
中级
1 day
说明
1
1
Dissolve the aniline
Dissolve the aniline
Dissolve 1 part by weight of aniline in about 5 parts of ether at room temperature.
此步骤所需材料：
苯胺1 part by weight所需工具：
乙醚
圆底烧瓶
等臂天平2
2
Add diketene slowly
Add diketene slowly
Add 1 part of diketene slowly with stirring. Keep it at room temperature or a little above, never even locally above 80-100 C; cool if needed.
此步骤所需材料：
乙烯酮二聚体1 part by weight所需工具：
带活塞的分液漏斗
温度计3
3
Let it crystallise
Let it crystallise
When the reaction is over, let the liquid stand; acetoacetanilide crystallises.
所需工具：
圆底烧瓶4
4
Collect and wash
Collect and wash
Decant or filter off the crystals and wash them with a little cold ether.
所需工具：
布氏漏斗（瓷制）
滤纸乙醚此蓝图制作
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