HRID505323

反应详情

EQUATION

反应方程式

HRID 505323 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

Under an atmosphere of argon, a solution 2-amino-5-methylbenzamide (1.2 g, 80 mmol) in THF (25 ml) was added to a suspension of LiAlH4 (1.54 g, 40 mmol) in THF (25 ml) over 20 min. The suspension was heated to reflux (4 h). For workup, the mixture was cooled to 0° C., and 1.5 ml H2O, 3 ml 4n NaOH, and 3 ml H2O were added subsequently. The suspension was dried (Na2SO4), and evaporated under reduced pressure. The title compound (700 mg, 63%) was isolated from the residue by chromatographic purification (silica gel, CH2Cl2/MeOH (2M NH3)=9:1).

WORKUP

后处理

  1. temperatureThe suspension was heated
  2. temperatureto reflux (4 h)
  3. dry with materialThe suspension was dried (Na2SO4)
  4. customevaporated under reduced pressure