HRID1666102

反应详情

EQUATION

反应方程式

HRID 1666102 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

To a suspension of 6-methoxy-quinoline-4-carboxylic acid (prepared according to U.S. Pat. No. 5,338,851; 43.8 g, 215.6 mmol) in DMF (215 mL) were added K2CO3 (99%; 60.2 g, 431.2 mmol) and iodoethane (19.4 mL, 237.2 mmol). The mixture was heated at 55° C. overnight. The solvent was evaporated to dryness, and the residue was partitioned between EA (1.5 L) and water (600 mL). The org. layer was washed twice with brine (2×300 mL), dried over Na2SO4, filtered and concentrated to dryness to yield a purple solid (37.5 g).

WORKUP

后处理

  1. customprepared
  2. customThe solvent was evaporated to dryness
  3. customthe residue was partitioned between EA (1.5 L) and water (600 mL)
  4. washlayer was washed twice with brine (2×300 mL)
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated to dryness