HRID1248133

反应详情

EQUATION

反应方程式

HRID 1248133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The ketone produced as described above (37.0 g) and 98% formic acid (9 ml) were added to formamide (23.5 ml) at 170° C. and the temperature kept at 175°-180° C. for five hours. A further portion of formic acid (4.5 ml) was added and the mixture was maintained at 175°-180° C. for a further fifteen hours. The mixture was extracted with ether which on evaporation gave a thick oil which was crystallised from petroleum ether (b.p. 60°-80°) to give N-formyl-1-[1-(3,4-dichlorophenyl)cyclobutyl]butylamine havng a melting point of 103°-105° C. (Formula I R1 =propyl; R2 =H; R3 =H; R4 =CHO; R5 =4-Cl and R6 =3-Cl).

WORKUP

后处理

  1. temperaturethe mixture was maintained at 175°-180° C. for a further fifteen hours
  2. extractionThe mixture was extracted with ether which on evaporation
  3. customgave a thick oil which
  4. customwas crystallised from petroleum ether (b.p. 60°-80°)