Phentolamine mesilate synthesis
- Product Name:Phentolamine mesilate
- CAS Number:65-28-1
- Molecular formula:C18H23N3O4S
- Molecular Weight:377.46
Yield:65-28-1 99%
Reaction Conditions:
in ethanol; pH=5 - 6;
Steps:
1 Example 1
Example 1
B salt formation: _: b1) Add 240mmL anhydrous ethanol and 24g phentolamine free base to 400mmL beaker. After stirring using a glass rod until dissolved, slowly stir while adding dropwise, methanesulfonic acid + ethanol solution until pH=7 (approximately 8.2 g methanesulfonic acid is needed to be added) then use an accurate pH test paper to adjust pH to 5-6.
Filter twice. Place filtrate in 500mm three-necked flask. Distill under vacuum using water bath (water bath temp below 55). Concentrate ethanol to about 1/3. When the inside of the bottle shows thick syrup, finish with vacuum disitllation.
In the flask, add equal volume of ethyl acetate (about 95mml). Scrape off solid from the walls of the bottle using a scraper. Shake to precipitate off crystals. Refrigerate, away from light, at 10-15 for 6h. Filter. Wash, 2-3times, using ethyl acetate. Drain. Dry at 80 for 6h. Obtain about 27g of white mesylate phentolamine. Purity is greater then 99%. mp176.5-181pH=5-6chlorine eligible; including bacterial test
References:
CN103408495,2016,B Location in patent:Paragraph 033; 0034; 0035; 0036
1634-04-4
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65-28-1
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