反应 #340910

反应方程式

4-Aminobutyric acid

phosphorous acid

Phosphorus trichloride

→

product

收率 43.1%

Alendronic Acid

收率 43.1%

溶剂

n-octane

反应条件

后处理

1. 1
   其他fitted with an addition funnel, mechanical stirrer, condenser
2. 2
   温度to heat at 90-95° C
3. 3
   温度The reaction mixture was cooled
4. 4
   workup.DISTILLATIONdistilled water (500 mL)
5. 5
   workup.ADDITIONwas added to it
6. 6
   温度The reaction mixture was further heated to 90-95° C
7. 7
   温度It was then cooled
8. 8
   workup.ADDITIONethanol (1000 mL) was added to it
9. 9
   温度The solution was further cooled to 0-5° C.
10. 10
    workup.STIRRINGstirred for 4-5 hrs
11. 11
    过滤The precipitated solid was filtered
12. 12
    洗涤washed with ethanol
13. 13
    其他dried under vacuum

实验过程

4-Aminobutyric acid (50 gm), phosphorous acid (140 gm) and n-octane (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 (240 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 ethanol (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 and washed with ethanol and dried under vacuum to yield 52.0 gm product.

来源