HRID1294564

反应详情

EQUATION

反应方程式

HRID 1294564 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

676.3 mg (17.8 mmol) lithium aluminium hydride are placed in 65 ml diethyl ether under an N2 atmosphere and cooled to 0° C. 2.01 g (11.9 mmol) methyl 2-amino-6-fluoro-benzoate, dissolved in 65 ml diethyl ether, are slowly added dropwise thereto and the mixture is stirred for 2 h at 0° C. Then the reaction mixture is combined dropwise at 0° C. with 100 ml dist. H2O. The aqueous phase is extracted twice with 100 ml diethyl ether. The combined organic phases are washed once with 100 ml of a saturated, aqueous NaCl solution, dried with MgSO4 and the solvent is eliminated in vacuo.

WORKUP

后处理

  1. additionare slowly added dropwise
  2. customis combined dropwise at 0° C. with 100 ml dist
  3. extractionThe aqueous phase is extracted twice with 100 ml diethyl ether
  4. washThe combined organic phases are washed once with 100 ml of a saturated, aqueous NaCl solution
  5. dry with materialdried with MgSO4