Acetic Acid → Etidronic Acid

Temperature

92.5 °C

Acetic acid (50 g), phosphorous acid (240 gm) and 1,4-dioxane (1000 mL) was taken in a four necked round bottom flask fitted with an addition funnel, mechanical stirrer, condenser and thermometer pocket and allowed to stir at 90-95° C. Phosphorus trichloride (400 gm) was then added to the reaction mixture and allowed to heat at 90-95° C. The reaction mixture was cooled and distilled water (500 ml) was added to it. The reaction mixture was further heated to 90-95° C. It was then cooled and acetonitrile (1000 mL) was added to it. The solution was further cooled to 0-5° C. and stirred for 4-5 hrs. The precipitated solid was filtered, washed with acetonitrile and dried in vacuum oven to give 9 gm of product.

1. customfitted with an addition funnel, mechanical stirrer, condenser
2. temperatureto heat at 90-95° C
3. temperatureThe reaction mixture was cooled
4. distillationdistilled water (500 ml)
5. additionwas added to it
6. temperatureThe reaction mixture was further heated to 90-95° C
7. temperatureIt was then cooled
8. additionacetonitrile (1000 mL) was added to it
9. temperatureThe solution was further cooled to 0-5° C.
10. stirringstirred for 4-5 hrs
11. filtrationThe precipitated solid was filtered
12. washwashed with acetonitrile
13. customdried in vacuum oven

ORD record

ord-dd6be1d4050543ef93c27a7f12373449

Source dataset

uspto-grants-2011_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07872144B2