HRID335190

反应详情

EQUATION

反应方程式

HRID 335190 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl 5-bromo-4-oxopentanoate (2.51 g, 12.0 mmol), 1-(5-bromo-3-phenoxypyridin-2-yl)thiourea (3.00 g, 9.25 mmol), triethylamine (2.19 mL, 15.7 mmol), and ethanol (60 mL) was refluxed for 3 hours and then stirred at ambient temperature overnight. The solvent was removed to about one third original volume and partitioned between CH2Cl2 and water. The organics were concentrated and purified on silica gel eluting with 40% EtOAc/Hexanes to give the title compound (3.22 g, 80.1% yield).

WORKUP

后处理

  1. temperaturewas refluxed for 3 hours
  2. customThe solvent was removed to about one third original volume
  3. custompartitioned between CH2Cl2 and water
  4. concentrationThe organics were concentrated
  5. custompurified on silica gel eluting with 40% EtOAc/Hexanes