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
2-Methylheptan-2-ol (56.53 g.; 0.43 mole) and phthalimidoacetonitrile (80.27 g.; 0.43 mole) were dissolved in glacial acetic acid (220 ml.) and the solution warmed to about 60° C. with stirring. Concentrated sulphuric acid (59 ml.; 1.1 mole) was then added gradually; at first the temperature fell but as the addition proceeded a vigorous exothermal reaction took place, the temperature of the reaction was controlled at 70° C. by regulating the addition of the sulphuric acid and coolingas necessary. When the addition was complete the resulting dark brown solution was stirred for 11/2 hours and then added dropwise to a mixture of ice and water. The precipitated solid was filtered off, pressed well, washed with fresh water and dried in vacuo. The residue was recrystallisedfrom benzene with filtering, to afford 2-phthalimido-N-(1,1-dimethylhexyl)acetamide m.p. 142° C.
WORKUP
后处理
- additionat first the temperature fell but as the addition
- customa vigorous exothermal reaction
- customwas controlled at 70° C.
- additionWhen the addition
- stirringwas stirred for 11/2 hours
- filtrationThe precipitated solid was filtered off
- washwashed with fresh water
- customdried in vacuo
- filtrationwith filtering