تفاعل #52596

معادلة التفاعل

Chloral hydrate

hydroxylamine hydrochloride

4-anisidine

hydrochloric acid

→

N-(2-hydroximino-acetyl)anisidine

المردود 85.2%

المذيبات

water

sodium sulfate

water

water

ظروف التفاعل

المعالجة

1. 1
   أخرىwas held at 60° C
2. 2
   workup.ADDITIONThe first solution was added to the second and the mixture
3. 3
   درجة الحرارةrefluxed for 2 minutes after which it
4. 4
   درجة الحرارةwas cooled slowly to room temperature
5. 5
   درجة الحرارةcooled in an ice bath
6. 6
   ترشيحThe tan precipitate was collected by vacuum filtration
7. 7
   غسيلwashed with water
8. 8
   أخرىdried under vacuum

الإجراء التجريبي

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.

المصدر