HRID1791948

反应详情

EQUATION

反应方程式

HRID 1791948 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Bromine (2.32 mL) was dissolved in 5% aqueous potassium hydroxide solution (190 mL), and a solution of 4-chloroquinoline-2-carboxamide [product of Example 262 (1), 9.80 g] in tetrahydrofuran (190 mL) was dropwise added thereto. The mixture was stirred at room temperature for 30 min, and the mixture was stirred at 80° C. for 1 hr with heating. The reaction mixture was filtrated and the filtrate was added to water. The mixture was extracted with chloroform, and the extract was washed with brine and concentrated under reduced pressure. The residue was purified by silica gel chromatography to give 2-amino-4-chloroquinoline (1.98 g) as a pale-yellow solid.

WORKUP

后处理

  1. stirringthe mixture was stirred at 80° C. for 1 hr
  2. temperaturewith heating
  3. filtrationThe reaction mixture was filtrated
  4. additionthe filtrate was added to water
  5. extractionThe mixture was extracted with chloroform
  6. washthe extract was washed with brine
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by silica gel chromatography