反応 #48483

反応方程式

Methanesulphonic acid

1H-Indole-3-carboxylic acid 10-oxo-8-aza-tricyclo[5.3.1.03,8]undec-5-yl ester

→

1H-Indole-3-carboxylic acid 10-oxo-8-aza-tricyclo[5.3.1.03,8]undec-5-yl ester methanesulphonate monohydrate

収率 148.8%

溶媒

acetone

反応条件

後処理

1. 1
   workup.WAITat room temperature for one night
2. 2
   ろ過the solid that forms is filtered
3. 3
   洗浄washed with acetone
4. 4
   その他The product formed
5. 5
   その他is recrystallised from isopropanol-water (95:5 by weight)

実験手順

Methanesulphonic acid (0.34 mL, 5.24 mmol) is added to a solution of 1H-Indole-3-carboxylic acid 10-oxo-8-aza-tricyclo[5.3.1.03,8]undec-5-yl ester (1.6 gr, 4.93 mmol) in acetone (20 mL) and under nitrogen, maintaining the reaction temperature around 25° C. Following stirring at 0° C. for 3 h, and at room temperature for one night, the solid that forms is filtered and washed with acetone. The product formed is recrystallised from isopropanol-water (95:5 by weight), to obtain 1H-Indole-3-carboxylic acid 10-oxo-8-aza-tricyclo[5.3.1.03,8]undec-5-yl ester methanesulphonate monohydrate (1.71 gr, 79%) in the form of a white solid.

出典