HRID1032303

反应详情

EQUATION

反应方程式

HRID 1032303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1155 g (6.4 mol) of 6-chloro-3,4-dihydro-2(1H)-naphthalenone were dissolved in 5 1 of toluene, 500 g (7.0 mol) of pyrrolidine and subsequently a solution of 26 g (0.14 mol) of p-toluenesulphonic acid in toluene were added dropwise thereto and the mixture was boiled under reflux When about 120 ml of water had separated, 4 1 of toluene were distilled off and the mixture was left to cool slowly. A solid crystallized out. Filtration and washing with acetone gave 1-(6-chloro-3,4-dihydro-2-naphthyl)pyrrolidine of melting point 117°-118°. Concentration of the mother liquor, suspension of the residue in ether, filtration and washing with acetone gave a further portion of the above product of melting point 117°-118°.

WORKUP

后处理

  1. customhad separated
  2. distillation4 1 of toluene were distilled off
  3. waitthe mixture was left
  4. temperatureto cool slowly
  5. customA solid crystallized out
  6. filtrationFiltration
  7. washwashing with acetone