HRID1958010

反应详情

EQUATION

反应方程式

HRID 1958010 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of lithium aluminium hydride (29.8 mL, 29.8 mmol) in THF was cooled to 0° C., and a solution of methyl 3-chloro-2-methylbenzoate (2.5 g, 13.54 mmol) in Tetrahydrofuran (THF) (20 mL) was added dropwise. The mixture was stirred at 0° C. for half hour, warmed up to RT gradually, and stirred at RT for 2 hours. Water and 6N NaOH (4 ml) were added to quench the reaction. The mixture was filtered and the filtrate was concentrated to afford the crude product as a white solid (2.0 g, 94%). 1H NMR (400 MHz, CDCl3) δppm 7.30˜7.35 (m, 2H), 7.16 (m, 1H), 4.74 (s, 2H), 2.40 (s, 3H).

WORKUP

后处理

  1. temperaturewarmed up to RT gradually
  2. stirringstirred at RT for 2 hours
  3. customto quench
  4. customthe reaction
  5. filtrationThe mixture was filtered
  6. concentrationthe filtrate was concentrated