HRID1194444

反应详情

EQUATION

反应方程式

HRID 1194444 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of the ketone produced as described above (21 g) and 98% formic acid (6 ml) was added over a period of one and a half hours to formamide (15 ml) at 160° C. After completion of the addition the temperature was raised to 180° to 185° C. and maintained in this range for five hours. The mixture was cooled and extracted with chloroform to yield a thick gum which on heating with petroleum ether (b.p. 60°-80°) gave a colourless solid which was recrystallised from petroleum ether (b.p. 60°-80°) to yield N-formyl-1-[1-(4-chlorophenyl)cyclobutyl]butylamine (m.p. 97.5° to 98.5° C.) (Formula I R1 =propyl; R2 =H; R3 =H; R4 =CHO; R5 =4-Cl; R6 =H).

WORKUP

后处理

  1. customproduced
  2. additionAfter completion of the addition the temperature
  3. temperaturewas raised to 180° to 185° C.
  4. temperaturemaintained in this range for five hours
  5. temperatureThe mixture was cooled
  6. extractionextracted with chloroform
  7. customto yield a thick gum which
  8. customgave a colourless solid which
  9. customwas recrystallised from petroleum ether (b.p. 60°-80°)