HRID434375

反应详情

EQUATION

反应方程式

HRID 434375 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Trimethylsilyl cyanide (8.5 g) was added to a stirred mixture of 2-fluorobenzaldehyde (10.6 g) and zinc iodide (500 mg) in dry ether (150 ml). The mixture was stirred at ambient temperature for 24 hours and was then added dropwise to a stirred suspension of lithium aluminium hydride (3.2 g) in dry ether (50 ml) under nitrogen. The mixture was refluxed for 2 hours, cooled and water (3.2 ml), 2 N sodium hydroxide solution (3.2 ml) and water (9.6 ml) slowly added. The precipitate was filtered off, the filtrate was dried (MgSO4) and evaporated to a yellow oil (13.0 g) which crystallised slowly on standing.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 2 hours
  2. temperaturecooled
  3. filtrationThe precipitate was filtered off
  4. dry with materialthe filtrate was dried (MgSO4)
  5. customevaporated to a yellow oil (13.0 g) which
  6. customcrystallised slowly