ChemicalBook CAS DataBase List NERIDRONATE SODIUM HYDRATE

NERIDRONATE SODIUM HYDRATE synthesis

5synthesis methods

Product Name:NERIDRONATE SODIUM HYDRATE
CAS Number:79778-41-9
Molecular formula:C6H17NO7P2
Molecular Weight:277.15

6- Aminohexanoic acid (152) was reacted with phosphorus trichloride and phosphorous acid at 85°C, and then water was added to generate free diphosphonic acid 16 in 78% overall yield [59].

60-32-2 Synthesis

60-32-2
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79778-41-9
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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]