反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
A suspension of phthalimidoacetonitrile (6.01 g, 0.03 mole) in glacial acetic acid (16 ml) was heated to 60° C. with stirring; 2,6-dimethylheptan-2-ol (4.64 g, 0.03 mole) was then added followed dropwise by concentrated sulphuric acid (4.4 ml, 0.08 mole). The temperature rapidly rose to 20° and was controlled at this temperature during the addition. When the addition was complete the solution was stirred for 5 minutes and then added slowly to a mixture of ice and water (350 g). The precipitated solid was filtered off, washed thoroughly with water and dried in vacuo. The product was recrystallised from benzene with filtering to afford 2-phthalimido-N-(1,1,5-trimethylhexyl)acetamide, m.p. 162°-163°.
WORKUP
后处理
- customrapidly rose to 20°
- additionwas controlled at this temperature during the addition
- additionWhen the addition
- stirringwas stirred for 5 minutes
- filtrationThe precipitated solid was filtered off
- washwashed thoroughly with water
- customdried in vacuo
- customThe product was recrystallised from benzene
- filtrationwith filtering