利塞膦酸 → 利噻膦酸钠

HRID 217110笔记

反应方程式

HRID 217110 反应方程式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][C:8]([OH:17])([P:13]([OH:16])(=[O:15])[OH:14])[P:9]([OH:12])(=[O:11])[OH:10])[CH:2]=1.[OH-:18].[Na+:19]>O>[CH:5]1[CH:6]=[N:1][CH:2]=[C:3]([CH2:7][C:8]([P:9]([O-:11])([OH:12])=[O:10])([P:13]([OH:16])([OH:15])=[O:14])[OH:17])[CH:4]=1.[CH:5]1[CH:6]=[N:1][CH:2]=[C:3]([CH2:7][C:8]([P:9]([O-:11])([OH:12])=[O:10])([P:13]([OH:16])([OH:15])=[O:14])[OH:17])[CH:4]=1.[OH2:18].[OH2:10].[OH2:10].[OH2:10].[OH2:10].[Na+:19].[Na+:19]

参与物

4

反应物 2

HCID 5245利塞膦酸HCID 14798氢氧化钠

产物 1

HCID 11954322利噻膦酸钠收率 194.1%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

反应条件

温度
25 °C

实验过程

To 60 ml of purified water, 10.0 g of 2-(3-pyridyl)-1-hydroxyethane-1,1-bisphosphonic acid (risedronic acid) and 1.41 g of sodium hydroxide were added and dissolved at an elevated temperature of 65° C. After the dissolution, the resulting solution was cooled to 25° C. over 3 hours for crystallization. The obtained crystals were filtered and vacuum dried to obtain 8.0 g of risedronate sodium hemipentahydrate (64.7% of theoretical yield). (LOD by TGA=13.2%)

后处理

  1. dissolutiondissolved at an elevated temperature of 65° C
  2. dissolutionAfter the dissolution
  3. filtrationThe obtained crystals were filtered
  4. customvacuum dried

来源与证据

ORD记录
ord-9e6beb172792440a92180700437b9fb4
来源数据集
uspto-grants-2012_06
专利号
US08193355B2

反应笔记

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