反応 #65986

反応方程式

SnCl2

sodium nitrite

4-benzyloxyaniline

→

product

収率 95.0%

4-Benzyloxyphenylhydrazine hydrochloride

収率 95.0%

溶媒

HCl

反応条件

後処理

1. 1
   workup.STIRRINGThe reaction mixture is stirred for 90 minutes at -8° to 10° C
2. 2
   workup.STIRRINGstirred for i hour at 0° C
3. 3
   その他The reaction mixture is removed from the ice bath
4. 4
   workup.STIRRINGis stirred at room temperature for 20 hours
5. 5
   ろ過The mixture is then filtered
6. 6
   洗浄washed with water

実験手順

A solution of sodium nitrite (3.8 g, 0.055 mol in 20 mL of H2O), is added dropwise to an ice cold stirring suspension of 4-benzyloxyaniline (13.0 g, 0.055 mol in 150 mL of concentrated HCl). The reaction mixture is stirred for 90 minutes at -8° to 10° C. A solution of SnCl2 ·2H2O (32.0 g, 0142 mol in 50 mL concentrated HCl) is added and stirred for i hour at 0° C. The reaction mixture is removed from the ice bath and is stirred at room temperature for 20 hours. The mixture is then filtered and washed with water to give 13.0 g (95% yield) of product, m.p. 182°-185° C.

出典