反应详情

2.383 mg of L-malic acid was added to 0.55 ml of a solution of 1-(2-fluorophenyl)-3-(piperidin-4-yloxy)-1H-indazole in MeOH (concentration=10.3 mg/ml). The solution was heated and stirred in uncapped vials and then placed under a stream of N2 gas. These steps were repeated until approximately 0.100 ml or less of solution remained. Approximately 0.500 ml of MTBE was then added. Precipitation was observed and the suspension was capped and stirred for 3 hours or less. Spheres of gel were observed and no solid was seen. The vial was then uncapped and allowed to stir for approximately 16 hours. A dry white solid remained. Subsequent attempts at repeating this procedure on a larger scale did not generate solid material.

1. temperatureThe solution was heated
2. customPrecipitation
3. customthe suspension was capped
4. stirringstirred for 3 hours or less
5. stirringto stir for approximately 16 hours