HRID271830

反应详情

EQUATION

反应方程式

HRID 271830 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 3-benzyl-2,7-dichloroquinoline (3.0 g, 10.4 mmol) and sodium iodide (15.6 g, 104 mmol) in 30 mL of methyl ethyl ketone was heated to 80° C. To this was added hydroiodic acid (1.13 ml, 13.2 mmol). The reaction mixture was heated at 80° C. for 1.5 hours and then cooled to ambient temperature. The reaction was quenched with H2O. Excess ethyl acetate was added to the reaction mixture and the organic layer was washed with saturated NaHCO3, saturated Na2S2O3, brine, dried over MgSO4, filtered and the solvent was removed in vacuo to yield 3.9 g (10.3 mmol, 99%) of 3-benzyl-7-chloro-2 iodo-quinoline 23 as a tan solid.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated at 80° C. for 1.5 hours
  2. temperaturecooled to ambient temperature
  3. customThe reaction was quenched with H2O
  4. additionExcess ethyl acetate was added to the reaction mixture
  5. washthe organic layer was washed with saturated NaHCO3, saturated Na2S2O3, brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customthe solvent was removed in vacuo