Risedronic acid synthesis
- Product Name:Risedronic acid
- CAS Number:105462-24-6
- Molecular formula:C7H11NO7P2
- Molecular Weight:283.11
6419-36-9
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105462-24-6
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$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%
References:
FLEMING LABORATORIES LIMITED WO2009/34580, 2009, A1 Location in patent:Page/Page column 7
501-81-5
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105462-24-6
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120067-55-2
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105462-24-6
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17747-43-2
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105462-24-6
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6419-36-9
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10294-56-1
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105462-24-6
288 suppliers
$7.00/1g