反応 #1994316

反応方程式

hydrochloric acid

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

hydrogen peroxide

→

desired product

6-amino-5-methyl-1H-indazole-7-carboxylic acid

溶媒

sodium hydroxide

反応条件

後処理

1. 1
   温度maintaining the temperature <30° C. with external cooling
2. 2
   その他The resulting reaction mixture
3. 3
   workup.WAITthe reaction was complete after 2 hours
4. 4
   ろ過The resulting brown suspension was filtered
5. 5
   洗浄the filtercake washed with cold water
6. 6
   その他dried in vacuo at 50° C.

実験手順

To a solution of 5-methyl-1,6-dihydro-pyrrolo[2,3-g]indazole-7,8-dione (23 g, 114.3 mmol) in 4N aqueous sodium hydroxide solution (160 ml) at ambient temperature, was added dropwise 30% aqueous hydrogen peroxide solution (27 ml) maintaining the temperature <30° C. with external cooling. The resulting reaction mixture was stirred at ambient temperature for 2 hours. According to TLC, the reaction was complete after 2 hours. The pH was adjusted to pH 3.5 by addition of concentrated hydrochloric acid. The resulting brown suspension was filtered and the filtercake washed with cold water and dried in vacuo at 50° C. to afford the desired product as brown solid. LC/MS: 192 (M+H)+.

出典