HRID1094448

反应详情

EQUATION

反应方程式

HRID 1094448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a 1M solution of lithium aluminum hydride in THF (57 mL) at 0° C. is added a solution of 2-fluoro-5-methylbenzoic acid (8.0 g, 52 mmol) in 160 mL of ether drop-wise. The reaction is then heated at reflux for 1.5 hr. The reaction is then cooled to 0° C. and is quenched with H2O (4 mL), aqueous 40% NaOH (4 mL) and H2O (4 mL). The resultant slurry is then filtered through celite and MgSO4. The filtrate is then concentrated and purified by silica gel flash column chromatography to provide the title compound.

WORKUP

后处理

  1. temperatureThe reaction is then heated
  2. temperatureat reflux for 1.5 hr
  3. customis quenched with H2O (4 mL), aqueous 40% NaOH (4 mL) and H2O (4 mL)
  4. filtrationThe resultant slurry is then filtered through celite and MgSO4
  5. concentrationThe filtrate is then concentrated
  6. custompurified by silica gel flash column chromatography