HRID325873

反应详情

EQUATION

反应方程式

HRID 325873 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-formyl-2-[1-(4-chlorophenyl)cyclobutyl]-1-methylethylamine (11.06 g) prepared as described above was heated under reflux for six hours with a mixture of concentrated hydrochloric acid (34 ml), water (34 ml) and diethyleneglycoldimethyl ether (40 ml). The mixture was cooled, washed with ether and basified with aqueous sodium hydroxide. The basified solution was extracted into ether, washed with water, dried, evaporated and distilled to give 2-[1-(4-chlorophenyl)cyclobutyl]-1-methylethylamine (b.p. 119°-121° C. at 0.8 mm Hg). The amine (2.65 g) was dissolved in propan-2-ol (15 ml) and concentrated hydrochloric acid added to pH 2. Ether (110 ml) was added and crystals of 2-[1-(4-chlorophenyl) cyclobutyl]-1-methylethylamine hydrochloride (m.p. 184°-185° C.) were collected. (Formula I R1, R2 =H; R3, R4 =H; R5 =4-Cl; R6 =H; R7 =Me and R8 =H.)

WORKUP

后处理

  1. temperatureabove was heated
  2. temperatureThe mixture was cooled
  3. washwashed with ether and basified with aqueous sodium hydroxide
  4. extractionThe basified solution was extracted into ether
  5. washwashed with water
  6. customdried
  7. customevaporated
  8. distillationdistilled