HRID1649246

反应详情

EQUATION

反应方程式

HRID 1649246 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Ethyl 2-nitro-5-piperazinylcinnamate hydrochloride (3.5 g) was dissolved in a mixed solvent consisting of 150 ml of ethanol and 45 ml of water and the solution was adjusted to pH of about 7 with an aqueous sodium hydroxide. The solution was added 2 g of Raney nickel catalyst and placed in a glass autoclave followed by stirring at 80° C. under hydrogen gas pressure of 5 kg/cm2 for 4 hours. After removing hydrogen gas the reaction mixture was taken out and the catalyst was removed. The solution was concentrated to dryness and methanol was added to the residue to precipitate crystals, which then were collected by filtration and recrystallized from methanol to give 1.3 g of 6-(1-piperazinyl)-3,4-dihydrocarbostyril, m.p. 224°-231.5° C.

WORKUP

后处理

  1. customAfter removing hydrogen gas the reaction mixture
  2. customthe catalyst was removed
  3. concentrationThe solution was concentrated to dryness and methanol
  4. additionwas added to the residue
  5. customto precipitate crystals, which
  6. filtrationthen were collected by filtration
  7. customrecrystallized from methanol