HRID637437

反应详情

EQUATION

反应方程式

HRID 637437 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In one liter of acetic acid were dissolved 95 g of 5-acetamido-6-fluoroquinaldine. To this mixture were added 10 g of five percent platinum on charcoal. The mixture was hydrogenated with hydrogen gas at 30 psi on a Paar apparatus for five hours. The amount of hydrogen used was 61 psi (verus 62 psi theoretical). The catalyst was removed by filtration, and the filtrate was concentrated to 250 ml and decanted into cold stirred sodium hydroxide solution. The white precipitate was separated by filtration and triturated with a chloroform/hexane (50/50) mixture to provide white crystals of 5-acetamido-6-fluorotetrahydroquinaldine, m.p. 168°-170° C. The structural assignment was confirmed by infrared spectral analysis.

WORKUP

后处理

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated to 250 ml
  3. customdecanted
  4. customThe white precipitate was separated by filtration
  5. customtriturated with a chloroform/hexane (50/50) mixture