HRID1277485

反应详情

EQUATION

反应方程式

HRID 1277485 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customrapidly rose to 20°
  2. additionwas controlled at this temperature during the addition
  3. additionWhen the addition
  4. stirringwas stirred for 5 minutes
  5. filtrationThe precipitated solid was filtered off
  6. washwashed thoroughly with water
  7. customdried in vacuo
  8. customThe product was recrystallised from benzene
  9. filtrationwith filtering