HRID735692

反应详情

EQUATION

反应方程式

HRID 735692 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of ethyl 2-(4-bromophenyl)acetate (972 mg, 4 mmol) in 10 mL dry THF at −78° C. was added LDA (2 M, 2 mL, 4 mmol). The solution was warmed to rt and stirred 2 h, then was recooled to −78° C. EtI (0.52 mL) was added, then the reaction was stirred rt for 16 h. The reaction was quenched with sat. NH4Cl, then extracted with EtOAc (3×20 mL). The organic layer washed with brine, then dried (Na2SO4). Purification via flash chromatography (0-20% EtOAc in hexanes) gives 75A (228 mg, 21%). MS (ESI) m/z 271.0 (M+H)+.

WORKUP

后处理

  1. customwas recooled to −78° C
  2. stirringthe reaction was stirred rt for 16 h
  3. customThe reaction was quenched with sat. NH4Cl
  4. extractionextracted with EtOAc (3×20 mL)
  5. washThe organic layer washed with brine
  6. dry with materialdried (Na2SO4)
  7. customPurification via flash chromatography (0-20% EtOAc in hexanes)