反応 #216159
ord-bf33a29f5886453aae83781a0538dfb4
反応方程式
反応物
試薬
なし
反応条件
温度
-5°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1workup.STIRRING' stirring at room temperature
- 2その他The solution was evaporated in vacuo
- 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).