反応 #52596

反応方程式

Chloral hydrate

hydroxylamine hydrochloride

4-anisidine

hydrochloric acid

→

N-(2-hydroximino-acetyl)anisidine

収率 85.2%

溶媒

water

sodium sulfate

water

water

反応条件

後処理

1. 1
   その他was held at 60° C
2. 2
   workup.ADDITIONThe first solution was added to the second and the mixture
3. 3
   温度refluxed for 2 minutes after which it
4. 4
   温度was cooled slowly to room temperature
5. 5
   温度cooled in an ice bath
6. 6
   ろ過The tan precipitate was collected by vacuum filtration
7. 7
   洗浄washed with water
8. 8
   その他dried under vacuum

実験手順

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.

出典