反応 #1994315

反応方程式

sulphuric acid

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

→

title product

5-methyl-1,6-dihydro-pyrrolo[2,3-g]indazole-7,8-dione

反応条件

後処理

1. 1
   workup.ADDITIONThe addition
2. 2
   workup.ADDITIONAt the end of the addition
3. 3
   その他the resulting reaction mixture
4. 4
   温度was heated at 80° C.
5. 5
   温度The reaction mixture was cooled down to ambient temperature
6. 6
   workup.STIRRINGThe resulting dark-brown suspension was stirred for 30 min
7. 7
   ろ過filtrated
8. 8
   洗浄The filter cake was washed extensively with water
9. 9
   その他dried in vacuo at 55° C

実験手順

To concentrated sulphuric acid (119 ml) was added portionwise 2-[(E)-hydroxyimino]-N-(5-methyl-1H-indazol-6-yl)-acetamide (34.7 g, 146.3 mmol). The addition was strongly exothermic and the internal temperature was maintained at 70° C. with an ice bath. At the end of the addition the resulting reaction mixture was heated at 80° C. and stirred for 45 min at this temperature. According to LC-MS analysis, the reaction has then reached completion. The reaction mixture was cooled down to ambient temperature. The reaction mixture was poured onto 3.00 kg of ice. The resulting dark-brown suspension was stirred for 30 min and then filtrated. The filter cake was washed extensively with water and dried in vacuo at 55° C. The title product was obtained as a red-brown powder. LC/MS: 202 (M+H)+, 224 (M+H)+.

出典