HRID425433

反应详情

EQUATION

反应方程式

HRID 425433 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A flask under nitrogen atmosphere was charged with CuI (2.77 g, 14.54 mmol) and ether (50 mL). The slurry was cooled to 0 C in an ice-water bath before a solution of MeLi in THF (1.6M, 18.2 mL, 29.1 mmol) was added dropwise over 20 minutes. A clear solution formed. A solution of methyl 4-bromocinnamate (3.19 g, 13.2 mmol) in THF (30 mL) was added dropwise via syringe over 30 minutes, and the resulting reaction mixture was stirred at 0 C for 2 hours. Then the reaction was quenched with ammonium chloride and worked up. The resulting crude product was purified by MPLC (0 to 15% ethyl acetate in hexanes) to afford methyl 3-(4-bromophenyl)butanoate.

WORKUP

后处理

  1. additionwas added dropwise over 20 minutes
  2. customA clear solution formed
  3. customthe resulting reaction mixture
  4. customThen the reaction was quenched with ammonium chloride
  5. customThe resulting crude product was purified by MPLC (0 to 15% ethyl acetate in hexanes)