Risedronate → Sodium hydrogen [1-hydroxy-1-phosphono-2-(pyridin-3-yl)ethyl]phosphonate

HRID 900386

반응식

HRID 900386 반응식
[OH-].[Na+:2].[CH:3]1[CH:8]=[N:7][CH:6]=[C:5]([CH2:9][C:10]([P:16]([OH:19])([OH:18])=[O:17])([P:12]([OH:15])([OH:14])=[O:13])[OH:11])[CH:4]=1.C(N(CC(O)=O)CC(O)=O)CN(CC(O)=O)CC(O)=O>O.C(O)C>[CH:3]1[CH:8]=[N:7][CH:6]=[C:5]([CH2:9][C:10]([P:12]([O-:14])([OH:15])=[O:13])([P:16]([OH:19])([OH:18])=[O:17])[OH:11])[CH:4]=1.[Na+:2]

참가 물질

5

반응물 3

HCID 5245RisedronateHCID 6049Ethylenediaminetetraacetic AcidHCID 14798Sodium Hydroxide

생성물 1

HCID 4194514Sodium hydrogen [1-hydroxy-1-phosphono-2-(pyridin-3-yl)ethyl]phosphonate수율 90%

시약·촉매·용매 1

HCID 19096565Water ethanol용매

반응 조건

온도
22 °C

실험 절차

A solution of sodium hydroxide (7.4 g, 1 eq.) in a mixture of water/ethanol (50%, v/v) (150 ml) was added dropwise to a suspension of risedronic acid (50 g) and 5 g of EDTA (ca. 10% on a dry per-weight basis) in a mixture of water/ethanol (50%, v/v) (850 ml) at reflux temperature. The reaction mixture was stirred at reflux temperature until the pH was stable at about 4.2-4.7. The reaction mixture was cooled to a temperature of about 22° C. The precipitate was then filtered, washed twice with 50 ml mixture of water/ethanol (50%, v/v) and then with ethanol (1×50 ml) and dried over night at 50° C. to give 48.5 g (85%) of sodium risedronate white crystal substance of form B (water content by thermogravimetric analysis was 5.5%-7.5%). Less than 50 ppm of iron was found in the produce by AES.

후처리

  1. customa dry per-weight basis)
  2. additionin a mixture of water/ethanol (50%, v/v) (850 ml)
  3. temperatureat reflux temperature
  4. temperatureat reflux temperature until the pH
  5. filtrationThe precipitate was then filtered
  6. washwashed twice with 50 ml mixture of water/ethanol (50%, v/v)
  7. dry with materialwith ethanol (1×50 ml) and dried over night at 50° C.

출처 및 근거

ORD 기록
ord-65188356dc534da9abf84fe1c0bd1ee0
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07358360B2

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