HRID494970

反应详情

EQUATION

反应方程式

HRID 494970 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

445 mg of 7-(2-(1,4-dioxa-8-azaspiro[4.5]decan-8-yl)ethyl)-6-methoxyquinoline was dissolved in 10 ml of methanol. Thereafter, 100 mg of 10% palladium carbon was added to the reaction solution. The obtained mixture was stirred for 6 hours under a 4 kg/cm2 of hydrogen atmosphere. Thereafter, palladium carbon was removed by filtration, and the filtrate was concentrated under a reduced pressure. The reaction solution was stirred under the same above conditions for 10 hours 3 times, and then, it was concentrated under a reduced pressure. A saturated sodium bicarbonate aqueous solution was added to the residue, followed by extraction with chloroform. The extract was dried over magnesium sulfate and then concentrated under a reduced pressure, so as to obtain 459 mg of 7-(2-(1,4-dioxa-8-azaspiro[4.5]decan-8-yl)ethyl)-6-methoxy-1,2,3,4-tetrahydroquinoline. This compound was used in the next reaction without further purification.

WORKUP

后处理

  1. customThereafter, palladium carbon was removed by filtration
  2. concentrationthe filtrate was concentrated under a reduced pressure
  3. concentrationit was concentrated under a reduced pressure
  4. additionA saturated sodium bicarbonate aqueous solution was added to the residue
  5. extractionfollowed by extraction with chloroform
  6. dry with materialThe extract was dried over magnesium sulfate
  7. concentrationconcentrated under a reduced pressure