ChemicalBook CAS DataBase List Risedronic acid

Risedronic acid synthesis

6synthesis methods

Product Name:Risedronic acid
CAS Number:105462-24-6
Molecular formula:C7H11NO7P2
Molecular Weight:283.11

6419-36-9
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$10.00/5g

105462-24-6
274 suppliers
$7.00/1g

Yield:105462-24-6 79.75%

Reaction Conditions:

Stage #1:3-pyridineacetic acid hydrochloride with phosphorous acid;phosphorus trichloride at 60 - 75; for 9 h;
Stage #2: with water at 25 - 95; for 8 h;

Steps:

1
3-pyridylacetic acid hydrochloride (100 gm, 0.576 moles) and phosphorous acid (103.97 gm, 1.267 moles) were taken in a four necked round bottom flask fitted on a water bath and stirred for ten minutes at ambient temperature (25⁰C to 3O⁰C). The reaction mixture was heated to 6O⁰C to 65⁰C and at this temperature phosphorous trichloride (198.12 gm, 1.44 moles) was added slowly in one hour to the reaction mixture. Then the reaction mixture was heated to 7O⁰C to 75⁰C and maintained for 8 hours at the same temperature. Reaction mixture was cooled to 55⁰C and the unreacted phosphorous trichloride was distilled at 5O⁰C to 55⁰C under vacuum. Water (725 ml) was added to the reaction mixture and heated at 9O⁰C to 95⁰C for six hours. Reaction mass was cooled to ambient temperature (25⁰C to 3O⁰C) and stirred for 2 hrs. Product is separated as crystalline solid, which was filtered, and dried at 43⁰C to 45⁰C under vacuum.Yield : 130 gms (79.75%) Purity (HPLC) : 99.83%