반응 #699524

반응 방정식

methyl 4-aminophenylacetate

NaNO2

SnCl2

→

18

수율 69.3%

methyl 4-hydrazinophenylacetate hydrochloride

수율 69.3%

용매

water

HCl

water

HCl

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture is vigorously stirred with a stirring rod
2. 2
   여과the resulting precipitate is collected by suction filtration
3. 3
   세척washed with water
4. 4
   기타The solid is dried under vacuum

실험 절차

To a solution of methyl 4-aminophenylacetate (5.5 g, 33.3 mmol) in concentrated HCl (35 mL) at 0° C. is added a solution of NaNO2 (2.3 g, 33.3 mmol) in water (10 mL). The temperature of the reaction is maintained at 0-5° C. After stirring for 30 minutes, a solution of SnCl2 (19 g, 99.9 mmol) in concentrated HCl (10 mL) is added and the mixture is vigorously stirred with a stirring rod. The mixture is then diluted with water (50 mL), and the resulting precipitate is collected by suction filtration and washed with water. The solid is dried under vacuum to give 5 g of 18, which is used without further purification.

출처