HRID1023202

反应详情

EQUATION

反应方程式

HRID 1023202 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 6-(2-hydroxyethoxy)-3,4-dihydroquinolin-2(1H)-one (0.15 g, 0.724 mmol) in DCM (2 mL) was added pyridine (0.117 mL, 1.448 mmol) and 4-methylbenzene-1-sulfonyl chloride (0.152 g, 0.796 mmol) and the reaction was stirred for 4 h. The reaction was diluted with EtOAc (25 mL), washed with 0.1 N HCl (10 mL), brine (10 mL), and sat. NaHCO3 solution (10 mL). The organic layer was dried over sodium sulfate, evaporated to dryness, and purified by flash chromatography on silica gel (4 g, 50% EtOAC in hexanes) to yield 2-(2-oxo-1,2,3,4-tetrahydroquinolin-6-yloxy)ethyl 4-methylbenzenesulfonate (0.07 g, 27%).

WORKUP

后处理

  1. washwashed with 0.1 N HCl (10 mL), brine (10 mL), and sat. NaHCO3 solution (10 mL)
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. customevaporated to dryness
  4. custompurified by flash chromatography on silica gel (4 g, 50% EtOAC in hexanes)