HRID1349990

反应详情

EQUATION

反应方程式

HRID 1349990 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl-6-ethylaminonicotinate in (59 mg, 0.332 mmol) DMF (0.8 mL) was added to sodium hydride (12 mg, 0.293 mL) in DMF (0.8 mL) at 0° C. The reaction was stirred for 1 hour and a solution of 2-(2-bromomethylphenyl sulfanylmethyl)benzene 5 (81 mg, 0.276 mmol) in 80 μL of DMF was added. The reaction was allowed to warm to ambient temperature and stirred for 18 hours. The solution was quenched with water and extracted with EtOAc (7×). The organic layers were combined, washed with water and brine twice, dried over MgSO4 and evaporated to give a white solid that was recrystallized from EtOAc/hexane. The solid was purified with 5% EtOAc/hexane by chromatography to yield 350 mg (70%) of the named compound.

WORKUP

后处理

  1. stirringstirred for 18 hours
  2. customThe solution was quenched with water
  3. extractionextracted with EtOAc (7×)
  4. washwashed with water and brine twice
  5. dry with materialdried over MgSO4
  6. customevaporated
  7. customto give a white solid
  8. customthat was recrystallized from EtOAc/hexane
  9. customThe solid was purified with 5% EtOAc/hexane by chromatography