HRID1445930

反应详情

EQUATION

反应方程式

HRID 1445930 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of NaH (98 mg, 2.5 mmol, 60% in mineral oil) in THF (10 mL), 4-methoxy-2-methyl-1H-pyrrolo[3,2-c]pyridine 3 (280 mg, 1.72 mmol) in THF (3 mL) was added. The mixture was stirred at room temperature for 30 min, and then 2-phenylbenzyl bromide (0.40 mL, 2.2 mmol) was added, stirring was continued for 18 h. The reaction mixture was quenched with saturated NH4Cl (20 mL), extracted with EtOAc (3×40 mL). The combined organic extracts were washed with water (40 mL), brine (40 mL), dried over Na2SO4 and evaporated. Flash chromatography of the residue over silica gel, using 10% EtOAc in hexanes to 25% EtOAc in hexanes) gave product 4 as a yellow foam. Yield: 375 mg (66%).

WORKUP

后处理

  1. additionwas added
  2. stirringstirring
  3. waitwas continued for 18 h
  4. customThe reaction mixture was quenched with saturated NH4Cl (20 mL)
  5. extractionextracted with EtOAc (3×40 mL)
  6. washThe combined organic extracts were washed with water (40 mL), brine (40 mL)
  7. dry with materialdried over Na2SO4
  8. customevaporated