HRID323495

反应详情

EQUATION

反应方程式

HRID 323495 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

Combine 1-(3,4,5-trimethoxybenzyl)-2-oxopyrrolidine (0.98 g, 3.70 mmol) and tetrahydrofuran (10 mL). Cool to −78° C. using a dry-ice/acetone bath. Add a solution of sec-butyl lithium (2.99 mL, 1.3 M in hexane, 3.88 mmol). After 30 minutes, add 4-fluorobenzyl bromide (0.70 g, 3.70 mmol). After the addition is complete, warm to ambient temperature. After 2 hours, add water and extract three times with ethyl acetate. Dry the combined organic layers over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Chromatograph the residue on silica gel eluting with ethyl acetate/hexane 1/1 to give the title compound.

WORKUP

后处理

  1. additionAfter the addition
  2. temperaturewarm to ambient temperature
  3. waitAfter 2 hours
  4. extractionextract three times with ethyl acetate
  5. dry with materialDry the combined organic layers over Na2SO4
  6. filtrationfilter
  7. concentrationconcentrate in vacuo
  8. customto obtain a residue