Sodium Hydroxide → Pantoprazole sodium (USP)

HRID 585775노트

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HRID 585775 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][N:6]=[C:7]([CH2:11][S+:12]([O-:26])[C:13]2[NH:14][C:15]3[CH:16]=[CH:17][C:18]([O:22][CH:23]([F:25])[F:24])=[CH:19][C:20]=3[N:21]=2)[C:8]=1[O:9][CH3:10].[OH-:27].[Na+:28].C([O:33]C)(C)(C)C>C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][N:6]=[C:7]([CH2:11][S:12]([C:13]2[N-:14][C:15]3[CH:16]=[CH:17][C:18]([O:22][CH:23]([F:24])[F:25])=[CH:19][C:20]=3[N:21]=2)=[O:26])[C:8]=1[O:9][CH3:10].[CH3:1][O:2][C:3]1[CH:4]=[CH:5][N:6]=[C:7]([CH2:11][S:12]([C:13]2[N-:14][C:15]3[CH:16]=[CH:17][C:18]([O:22][CH:23]([F:24])[F:25])=[CH:19][C:20]=3[N:21]=2)=[O:26])[C:8]=1[O:9][CH3:10].[OH2:33].[OH2:27].[OH2:2].[Na+:28].[Na+:28]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 15413tert-Butyl methyl etherHCID 178493214Pantoprazole

생성물 1

HCID 11954257Pantoprazole sodium (USP)

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
45 °C

실험 절차

Pantoprazole freebase (25 grams) was dissolved in a solution of ethyl acetate (50 ml) and aqueous sodium hydroxide solution (2.7 grams in 5 ml of water) and stirred at a temperature of 40-50° C. till the clear solution results. Methyl tertiary butyl ether (250 ml) was added to the reaction mixture and stirred for about 3-4 hours to crystallize the solid mass. The separated solid mass was filtered, washed with methyl tertiary butyl ether (50 ml) and suck dried under vacuum. The wet solid was further dried at a temperature of 40-50° C. to afford crystalline Form-I of Pantoprazole sodium sesquihydrate.

후처리

  1. customresults
  2. stirringstirred for about 3-4 hours
  3. customto crystallize the solid mass
  4. filtrationThe separated solid mass was filtered
  5. washwashed with methyl tertiary butyl ether (50 ml)
  6. customsuck dried under vacuum
  7. customThe wet solid was further dried at a temperature of 40-50° C.

출처 및 근거

ORD 기록
ord-43bdbdff25ab423cacdd26ba42ac6d59
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06933389B2

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