反応 #1994314

反応方程式

hydroxylamine hydrochloride

5-methyl-6-aminoindazol

sodium sulphate

chloralhydrate

→

desired product

2-[(E)-hydroxyimino]-N-(5-methyl-1H-indazol-6-yl)-acetamide

溶媒

hydrochloric acid

water

反応条件

後処理

1. 1
   その他The resulting reaction mixture
2. 2
   温度was heated-up gradually from ambient temperature to 80° C
3. 3
   その他an internal temperature of 80° C., it
4. 4
   温度The reaction mixture was then cooled down to ambient temperature with an ice bath
5. 5
   ろ過The reaction mixture was filtrated
6. 6
   洗浄The filtercake was washed thoroughly with water
7. 7
   その他dried at 50° C. for 15 hours

実験手順

To a solution of sodium sulphate (8.69 g, 61.15 mmol) in water (20 ml) was added chloralhydrate (0.62 g, 3.74 mmol) at ambient temperature. To the resulting clear solution was added a solution of 5-methyl-6-aminoindazol (0.5 g, 3.4 mmol, prepared as described in Eur. Pat. Appl. EP 040872) in 1N aqueous hydrochloric acid (3.7 ml). The resulting mixture turned cloudy and hydroxylamine hydrochloride (0.75 g, 10.9 mmol) was then added. The resulting reaction mixture was heated-up gradually from ambient temperature to 80° C. When the reaction mixture has reached an internal temperature of 80° C., it was stirred for an additional 30 min at 80° C. The reaction mixture was then cooled down to ambient temperature with an ice bath. The reaction mixture was filtrated. The filtercake was washed thoroughly with water and dried at 50° C. for 15 hours to afford the desired product as a brown powder of >95% purity according to HPLC. LC/MS: 219 (M+H)+.

出典