反応 #216159

ord-bf33a29f5886453aae83781a0538dfb4

反応条件

温度
-5°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRING' stirring at room temperature
  2. 2
    その他The solution was evaporated in vacuo
  3. 3
    その他the residue triturated with ether

実験手順

The product from step (b) (10.3 g) was suspended in water (53 ml) and c.HCl (106 ml) added dropwise. The resulting mixture was cooled to -5° C. and a solution of sodium nitrite (3.2 g) in water (30 ml) added dropwise to the stirred mixture over 15 minutes followed by 30 minutes' stirring at -5° to 0° C. The solution was then added at 0° C. over 15 minutes to a stirred solution of tin (II) chloride (51 g) in c.HCl (91 ml), followed by 3 hours' stirring at room temperature. The solution was evaporated in vacuo and the residue triturated with ether to give the desired product as a pale yellow solid (11 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05466699uspto-grants-1995_11