HRID1818219

反应详情

EQUATION

反应方程式

HRID 1818219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,5-Dimethoxytetrahydrofuran (1.6 mL of 95%, 12 mmol) was added to a suspension of 8-amino-1-(2-methylpropyl)-1H-imidazo[4,5-c]quinolin-4-amine (3.0 g, 12 mmol) in acetic acid (60 mL), and the reaction was heated at reflux for one hour. The resulting dark brown solution was concentrated under reduced pressure, and the residue was mixed with water. The resulting mixture was made basic with the addition of ammonium hydroxide and stirred for 30 minutes. The resulting precipitate was isolated by filtration, washed with water, dried, and recrystallized from ethanol (100 mL). The crystals were collected in three crops. The first crop was dried for a day in a vacuum oven at 100° C. to provide 2.1 g of 1-(2-methylpropyl)-8-(1-pyrrolyl)-1H-imidazo[4,5-c]quinolin-4-amine as a solid, mp 227.5-231.5° C.

WORKUP

后处理

  1. temperaturethe reaction was heated
  2. temperatureat reflux for one hour
  3. concentrationThe resulting dark brown solution was concentrated under reduced pressure
  4. additionthe residue was mixed with water
  5. additionThe resulting mixture was made basic with the addition of ammonium hydroxide
  6. customThe resulting precipitate was isolated by filtration
  7. washwashed with water
  8. customdried
  9. customrecrystallized from ethanol (100 mL)
  10. customThe crystals were collected in three crops
  11. customThe first crop was dried for a day in a vacuum oven at 100° C.