Sodium Hydroxide → Pantoprazole sodium (USP)

HRID 585775ノート

反応式

HRID 585775 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 11954257Pantoprazole sodium (USP)

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
45 °C

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-43bdbdff25ab423cacdd26ba42ac6d59
出典データセット
uspto-grants-2005_08
特許番号
US06933389B2

反応ノート

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