HRID1360561

反应详情

EQUATION

反应方程式

HRID 1360561 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Platinum (IV) oxide (4 g) was added to a solution of 1-(4-aminobutyl)-2-ethyl-2H-pyrazolo[3,4-c]quinolin-4-amine (approximately 24 mmol, prepared as described in Part A of Examples 349-453) in trifluoroacetic acid (80 mL), and the mixture was shaken under hydrogen pressure (50 psi, 3.4×105 Pa) for two days and subsequently filtered through a layer of CELITE filter agent. The filter cake was washed with methanol, and the filtrate was concentrated under reduced pressure. Water (10 mL) was added, and the resulting solution was adjusted to pH 14 with the addition of 50% aqueous sodium hydroxide. The resulting mixture was extracted with dichloromethane, and the extracts were dried over sodium sulfate, filtered, and concentrated under reduced pressure to provide 1-(4-aminobutyl)-2-ethyl-6,7,8,9-tetrahydro-2H-pyrazolo[3,4-c]quinolin-4-amine.

WORKUP

后处理

  1. customprepared
  2. filtrationsubsequently filtered through a layer of CELITE filter agent
  3. washThe filter cake was washed with methanol
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. additionWater (10 mL) was added
  6. additionthe resulting solution was adjusted to pH 14 with the addition of 50% aqueous sodium hydroxide
  7. extractionThe resulting mixture was extracted with dichloromethane
  8. dry with materialthe extracts were dried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure