HRID1277477

反应详情

EQUATION

反应方程式

HRID 1277477 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

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

  1. additionat first the temperature fell but as the addition
  2. customa vigorous exothermal reaction
  3. customwas controlled at 70° C.
  4. additionWhen the addition
  5. stirringwas stirred for 11/2 hours
  6. filtrationThe precipitated solid was filtered off
  7. washwashed with fresh water
  8. customdried in vacuo
  9. filtrationwith filtering