反应 #2314327

反应方程式

iso-pentylamine

diethyl DL-malate

diethyl DL-malate

iso-pentylamine

→

N,N′-Di-iso-pentyl DL-malamide

hexane

收率 100.0%

反应条件

后处理

1. 1
   其他to the removal of the excess amine under vacuum
2. 2
   温度with heating
3. 3
   其他A white waxy solid was obtained
4. 4
   其他The solid was triturated with hexane (4×100 mL)
5. 5
   过滤and the product was filtered through a glass frit after each trituration
6. 6
   其他Finally, the material was transferred to a round-bottomed flask
7. 7
   其他the white solid was dried under vacuum for one hour
8. 8
   温度while heating (<100° C.)

实验过程

N,N′-Di-iso-pentyl DL-malamide was prepared by the reaction of iso-pentylamine with diethyl DL-malate. To a round-bottomed flask were added diethyl DL-malate (20.013 g, 0.1052 mole, 1 eq) and iso-pentylamine (27.778 g, 3.03 eq). The clear light yellow solution was stirred for 20 hours at room temperature prior to the removal of the excess amine under vacuum with heating. A white waxy solid was obtained. The solid was triturated with hexane (4×100 mL); and the product was filtered through a glass frit after each trituration. Finally, the material was transferred to a round-bottomed flask and the white solid was dried under vacuum for one hour while heating (<100° C.) to remove any residual amine and hexane (28.99 g, ˜100% yield). The product was ˜100% pure as determined by NMR analyses.

来源