Methane → Pantoprazole sodium (USP)

HRID 2363800노트

반응식

HRID 2363800 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[N-: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].[Na+:27].C>CC(C)=O>[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].[OH2:2].[OH2:2].[OH2:2].[Na+:27].[Na+:27]

참가 물질

4

반응물 2

HCID 297MethaneHCID 178493213HCID 178493213, 화합물

생성물 1

HCID 11954257Pantoprazole sodium (USP)수율 212.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

Pantoprazole sodium (75 gms) as prepared according to Example-1 or Example-2 was dissolved in 375 ml of acetone at about 50-55° C., charcoal (5 gms) was added and the reaction mass was stirred for 15 minutes and clarified hot. The resulting clear filtrate was concentrated to approx. volume of 150 ml, ethyl acetate (400 ml) was added and distillation was continued until precipitation was observed in the reaction mass. The reaction mass was cooled to room temperature and water (4.2 ml) was added, the suspension was stirred for 1 hr. and later chilled and stirred at 0-5° C. for 1 hr. The product was the isolated by filtration and was dried at 40-45° C. under vacuum to give pantoprazole sodium sesquihydrate (68 gms.) having a moisture content of 6.5%.

후처리

  1. concentrationThe resulting clear filtrate was concentrated to approx. volume of 150 ml, ethyl acetate (400 ml)
  2. additionwas added
  3. distillationdistillation
  4. customwas continued until precipitation
  5. additionwater (4.2 ml) was added
  6. stirringthe suspension was stirred for 1 hr
  7. temperatureand later chilled
  8. stirringstirred at 0-5° C. for 1 hr
  9. customisolated by filtration
  10. customwas dried at 40-45° C. under vacuum

출처 및 근거

ORD 기록
ord-ba13252348cf42e68872dfc6d4edb7df
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08691995B2

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