تفاعل #985295

معادلة التفاعل

topiramate

sodium hydroxide

→

topiramate sodium

المردود 2.8%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added
2. 2
   workup.DISSOLUTIONto dissolve
3. 3
   ترشيحThe solution was filtered
4. 4
   أخرىevaporated at 60° C.
5. 5
   أخرىwas placed in a cold room (4° C.) overnight
6. 6
   ترشيحThe mixture was filtered
7. 7
   أخرىdried

الإجراء التجريبي

10.09 g (29.73 mmoles) of topiramate (Cheminor Drugs Ltd., Hyderabad, India, Batch TP001 J00) was placed in a 250 mL beaker and 100.0 mL of HPLC grade water (JT Baker, Phillipsburg, N.J. USA, Lot V32E17) was added. 1.36 g (34.0 mmoles) of sodium hydroxide (Sigma, St. Louis, Mo. USA, Lot 99H0120) was added and the mixture was stirred with a TEFLON® coated magnetic stir bar using a hot plate/stir plate. The mixture was heated to 60° C. to dissolve. The solution was filtered and evaporated at 60° C. while blowing air over the surface using a TYGON tube attached to an air source to reduce the volume to 15 mL, and the flask was placed in a cold room (4° C.) overnight. Crystals grew overnight. The mixture was filtered and dried to yield 305 mg topiramate sodium as large, block-like crystals. Elemental analysis: calc. C, 34.70, H, 6.31, N, 3.37%; found C, 34.90; H, 6.04; N, 3.36%. mp 80-85° C., recrystallization from melted material 110-120° C., second mp 170-175° C. PXRD Cu-Kα radiation (1.5406 Å) first 8 peaks (peak number/2Θ value), #1/4.51°, #2/12.09°, #3/12.709°, #4/13.67°, #5/15.01°, #6/16.17°, #7/17.19°, #8/17.55°. The pH of a 400 mg/mL solution of the compound in distilled water was about 11.2, which was determined using a Thermo Orion pH meter, Model 525A+ (Orion Research, Inc., Beverly, Mass. USA).

المصدر