NERIDRONATE SODIUM HYDRATE synthesis
- Product Name:NERIDRONATE SODIUM HYDRATE
- CAS Number:79778-41-9
- Molecular formula:C6H17NO7P2
- Molecular Weight:277.15
60-32-2
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Yield: 89%
Reaction Conditions:
Stage #1:6-aminohexanoic acid with phosphorus trichloride in methanesulfonic acid at 80 - 85;
Stage #2: with water in methanesulfonic acid at 105; for 4 h;
Steps:
3.2.1.Synthesisofamino-1-hydroxyalkan-1,1-diyl-bisphosphonicacids1-3
General procedure: Thesynthesisofaminobisphosphonicacidswasbasdonaliteraturemethod[84]somewhat modifiedbyus.Aportionoftheaminoacid(0.025mol)(β-alanine,γ-butanoicacid,ε-aminocaproic acid)isdissolvedin10mLofmethanesulfonicacid(MSA)inaflaskwithintensivestirring.Then,7.0 mL(0.080mol)ofphosphorus(III)chlorideisslowlyaddeddropwisetothesolutionover15min.The contentsoftheflaskarestirredunderheating(80-85°C)for4-6h,thencooledtoroomtemperature. Aftercooling,12mL(0.67mol)ofwaterareadded,andthereactionmixtureishydrolyzedat105°C for4h.Aftercooling,thepHofthesolutionisadjustedto6-7byaddingtothemixture12mLof50% aqueoussodiumhydroxidesolution.Thenthereactionmassprecipitatedwith40mLofMeOH.The precipitateisseparatedontheSchottfilter.Thecrudeproductisdissolvedin20mLofwater,stirredat 50-70°Cfor30min,thencooledandprecipitatedwith40mLofMeOH.Thesolidphaseisseparated usingaSchottfilter.
References:
Danilko, Ksenia V.;Dyakonov, Grigory S.;Farrakhov, Ruzil G.;Galimshina, Zulfia R.;Gil'fanova, Guzel U.;Lukina, Elena S.;Mukaeva, Veta R.;Parfenov, Evgeny V.;Parfenova, Lyudmila V. [Molecules,2020,vol. 25,# 1]
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1000210-73-0
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4443-26-9
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31968-60-2
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