Beta-Alanine → Pamidronic Acid
反応式
[P:1]([OH:4])([OH:3])[OH:2].[NH2:5][CH2:6][CH2:7][C:8]([OH:10])=O.N1CCOCC1.P(Cl)(Cl)Cl>>[CH2:7]([C:8]([P:1]([OH:4])([OH:3])=[O:2])([P:1]([OH:4])([OH:3])=[O:2])[OH:10])[CH2:6][NH2:5]参加物
5
反応条件
- 温度
- 70 °C
実験手順
The mixture of 5 eq. phosphorous acid and β-alanine is heated to form a melt. Morpholine (1 eq.) is slowly added. The reaction is cooled to about 70° C. and 2 eq. of PCl3 are added. The mixture is heated for about 3.5 hours. Then the reaction is hydrolyzed in aqueous acid at about 75° C. for about 0.5 hours. Crystallization from aqueous acid/IPA, affords pamidronate.
後処理
- temperatureis heated
- customto form a melt
- temperatureThe mixture is heated for about 3.5 hours
- customCrystallization from aqueous acid/IPA
出典と根拠
- ORDレコード
- ord-1073b756d7524ebf91ed74ed69b1f293
- 出典データセット
- uspto-grants-2003_05
- 特許番号
- US06562974B2
反応ノート
読み込み中…