HRID404677

反应详情

EQUATION

反应方程式

HRID 404677 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Lithium 2-(4-methoxyphenyl)-2-(piperidin-1-yl)acetate (384 mg, 1.50 mmol), DCC (621 mg, 3.01 mmol), and HOBT (461 mg, 3.01 mmol) were dissolved in dry THF (16 ml). (R)-quinuclidin-3-ol (574 mg, 4.51 mmol) was added and the mixture was stirred at room temperature for 16 hours. THF was evaporated and the crude was dissolved in EtOAc, washed with sat. NaHCO3, water and brine. The organic layer was dried over Na2SO4, filtered and evaporated. The crude was purified by flash chromatography (DCM/MeOH/NH4OH=9/1/0.02) to obtain (R)-quinuclidin-3-yl 2-(4-methoxyphenyl)-2-(piperidin-1-yl)acetate (207 mg, 38.4% yield) as a colourless oil.

WORKUP

后处理

  1. customTHF was evaporated
  2. dissolutionthe crude was dissolved in EtOAc
  3. washwashed with sat. NaHCO3, water and brine
  4. dry with materialThe organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. customevaporated
  7. customThe crude was purified by flash chromatography (DCM/MeOH/NH4OH=9/1/0.02)