HRID1450433

反应详情

EQUATION

反应方程式

HRID 1450433 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

Dissolve [2-benzothiazolyl][1-[2-(4-methoxyphenyl)ethyl]-4piperidinyl]methanone (2.0 g, 5.26 mmol) in anhydrous tetrahydrofuran (50 mL), place under an argon atmosphere and cool to -78° C. Add, by dropwise addition, phenyllithium (3.16 mL of a 2.0M solution in cyclohexane/ethyl ether, 6.31 mmol). Stir at -78° C. for 30 minutes, quench with saturated ammonium chloride (100 mL), separate the organic phase and extract the aqueous phase with ethyl acetate. Combine the organic phases, dry (MgSO4) and evaporate the solvent in vacuo. Purify by chromatography (75% ethyl acetate/hexane) to give a yellow oil. Dissolve the oil in methylene chloride and treat with activated charcoal.

WORKUP

后处理

  1. customquench with saturated ammonium chloride (100 mL)
  2. customseparate the organic phase
  3. extractionextract the aqueous phase with ethyl acetate
  4. dry with materialdry (MgSO4)
  5. customevaporate the solvent in vacuo
  6. customPurify by chromatography (75% ethyl acetate/hexane)
  7. customto give a yellow oil