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2-methyl-4-(4-methyl-1-piperazinyl)-10H-thieno[2,3-b][1,5]benzodiazepine preparation

IP.com Disclosure Number: IPCOM000023196D
Publication Date: 2004-Mar-29
Document File: 1 page(s) / 66K

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2-methyl-4-(4-methyl-1-piperazinyl)-10H-thieno[2,3-b][1,5] benzodiazepine

A crystalline anhydrous form of 2-methyl-4-(4-methyl-1-piperazinyl)-10H- thieno[2,3-b][1,5]benzodiazepine is prepared by drying of the wet hydrated crystalline 2-methyl-4-(4-methyl-1-piperazinyl)-10H-thieno[2,3-b][1,5]benzodiazepine.

Preparation of 2-methyl-4-(4-methyl-1-piperazinyl)-10H-thieno[2,3-b][1,5] benzodiazepine and its acid salts has been described in US Patent no. 5,229,382. Hydrated forms of crystalline 2-methyl-4-(4-methyl-1-piperazinyl)-10H-thieno[2,3-b] [1,5]benzodiazepine can be prepared according to the methods disclosed in e.g. US patent no. 6,020,487 and PCT publication no. WO 02/18390.

The process for drying of 2-methyl-4-(4-methyl-1-piperazinyl)-10H- thieno[2,3-b][1,5]benzodiazepine hydrate crystalline wet comprises 4 stages. In the first stage, the hydrate is dried for between about 2-7 hours at a temperature of about 21-29°C. In the second stage, the material is dried for between about 2-7 hours at a temperature of about 31-39°C. In the third stage, the material is dried for between about 2-7 hours at a temperature of about 46-54°C. In the fourth stage, the material is dried for between about 2-7 hours at a temperature of about 56-65°C. The drying is performed under a pressure of below 100mmHg. One would appreciate that any two stages would suffice to dry the wet hydrate.

Experiment for 2-methyl-4-(4-methyl-1-piperazinyl)-10H-thieno[2,3-b] [1,5]benzodiazepine drying T...