HRID1927251

反应详情

EQUATION

反应方程式

HRID 1927251 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a suspension of THF (40 mL) and LAH (2.4 g) was added aluminum chloride (9.7 g) at 0° C., which was stirred until the aluminum chloride dissolved. 4-((5-Chloro-furan-2-yl)-hydroxy-methyl)-benzonitrile (2.4 g) described in Manufacturing Example 16-1 was then added thereto at 0° C., which was stirred for 4 hours and 30 minutes at room temperature. An aqueous ammonia solution was added at 0° C. to the reaction suspension, which was filtered through Celite, and the solvent was evaporated from the filtrate under a reduced pressure. The residue was purified by NH silica gel column chromatography (heptane:ethyl acetate=1:2) to obtain the titled compound (1.6 g).

WORKUP

后处理

  1. dissolutiondissolved
  2. additionwas then added
  3. filtrationwas filtered through Celite
  4. customthe solvent was evaporated from the filtrate under a reduced pressure
  5. customThe residue was purified by NH silica gel column chromatography (heptane:ethyl acetate=1:2)