反応 #1179

反応方程式

NaNO2

SnCl2

4-amino-2,3-dimethylbenzoic acid

→

expected product

収率 93.7%

2,3-Dimethyl-4-hydrazinobenzoic acid hydrochloride

収率 93.7%

溶媒

water

HCl

HCl

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture is stirred for 30 minutes at -5° C.
2. 2
   その他2 hours
3. 3
   その他at RT
4. 4
   ろ過The mixture is filtered
5. 5
   洗浄the precipitate is washed with 5 ml of concentrated HCl
6. 6
   その他dried under a stream of dry nitrogen

実験手順

A solution of 1.87 g of NaNO2 in 7 ml of water is added slowly to a solution, cooled to -5° C., of 4.5 g of 4-amino-2,3-dimethylbenzoic acid in 135 ml of concentrated HCl. After 2 hours of stirring at -5° C., a solution of 25 g of SnCl2 ·2H2O in 250 ml of concentrated HCl is added at -10° C., and the mixture is stirred for 30 minutes at -5° C. and then 2 hours at RT. The mixture is filtered, and the precipitate is washed with 5 ml of concentrated HCl and dried under a stream of dry nitrogen and then under vacuum to obtain 5.5 g of expected product.

出典