Gamma-Aminobutyric Acid → Alendronic Acid

HRID 253728

反応式

HRID 253728 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][C:5]([OH:7])=O.[P:8]([OH:11])([OH:10])[OH:9].P(Cl)(Cl)Cl>CCCCCCCC>[CH2:3]([CH2:2][NH2:1])[CH2:4][C:5]([P:8]([OH:11])([OH:10])=[O:9])([P:8]([OH:11])([OH:10])=[O:9])[OH:7]

参加物

5

反応条件

温度
92.5 °C

実験手順

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.

後処理

  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. additionethanol (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 ethanol
  13. customdried under vacuum

出典と根拠

ORDレコード
ord-3e98a1a764f74a5698540f31dfd2bd9c
出典データセット
uspto-grants-2011_01
特許番号
US07872144B2

関連ノート

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