Reaktion #48483

Reaktionsgleichung

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

Ausbeute 148.8%

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITat room temperature for one night
2. 2
   Filtrationthe solid that forms is filtered
3. 3
   Waschenwashed with acetone
4. 4
   SonstigeThe product formed
5. 5
   Sonstigeis recrystallised from isopropanol-water (95:5 by weight)

Vorschrift

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.

Quelle