Reacción #52596

Ecuación de reacción

Chloral hydrate

hydroxylamine hydrochloride

4-anisidine

hydrochloric acid

→

N-(2-hydroximino-acetyl)anisidine

Rendimiento 85.2%

Disolventes

water

sodium sulfate

water

water

Condiciones de reacción

Tratamiento posterior

1. 1
   Otrowas held at 60° C
2. 2
   workup.ADDITIONThe first solution was added to the second and the mixture
3. 3
   Temperaturarefluxed for 2 minutes after which it
4. 4
   Temperaturawas cooled slowly to room temperature
5. 5
   Temperaturacooled in an ice bath
6. 6
   FiltraciónThe tan precipitate was collected by vacuum filtration
7. 7
   Lavadowashed with water
8. 8
   Otrodried under vacuum

Procedimiento

Chloral hydrate (9.6 g) was dissolved in 200 mL of water containing 83 g of sodium sulfate. The solution was warmed to 60° C., a solution of 11.4 g of hydroxylamine hydrochloride in 50 mL of water was added and the mixture was held at 60° C. In a separate flask, 6.4 g of 4-anisidine and 4.3 mL of concentrated hydrochloric acid in 80 mL of water was warmed to 80° C. The first solution was added to the second and the mixture refluxed for 2 minutes after which it was cooled slowly to room temperature and then cooled in an ice bath. The tan precipitate was collected by vacuum filtration, washed with water and dried under vacuum to give 8.6 g (85% yield) of N-(2-hydroximino-acetyl)anisidine.

Fuente