Acetic Acid → Pantoprazole

HRID 394827

반응식

HRID 394827 반응식
[F:1][CH:2]([F:25])[O:3][C:4]1[CH:24]=[CH:23][C:7]2[NH:8][C:9]([S:11][CH2:12][C:13]3[C:18]([O:19][CH3:20])=[C:17]([O:21][CH3:22])[CH:16]=[CH:15][N:14]=3)=[N:10][C:6]=2[CH:5]=1.C([O-])([O-])=[O:27].C([O-])([O-])=O.OO.OO.OO.[Na+].[Na+].[Na+].[Na+].O.C(O)(=O)C>CO.[NH4+].[NH4+].[O-][Mo]([O-])(=O)=O>[CH3:22][O:21][C:17]1[CH:16]=[CH:15][N:14]=[C:13]([CH2:12][S+:11]([O-:27])[C:9]2[NH:8][C:7]3[CH:23]=[CH:24][C:4]([O:3][CH:2]([F:1])[F:25])=[CH:5][C:6]=3[N:10]=2)[C:18]=1[O:19][CH3:20]

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 159762Sodium percarbonateHCID 9799341Pantoprazole sulfide

생성물 1

HCID 178493214Pantoprazole수율 204%

시약·촉매·용매 2

HCID 61578Diammonium molybdate촉매HCID 887Methanol용매

반응 조건

온도
20 °C

실험 절차

310 mg of 5-difluoromethoxy-2-[[(3,4-dimethoxy-2-pyridinyl)methyl]thio]-1H-benzimidazol were dissolved in 1.5 ml of methanol and 12 mg of ammonium molybdate added. The solution was cooled to 51C and 0.11 g of sodium percarbonate were added, then kept stirred at the same temperature for 4 h. After the reaction ended 3 ml of water were added, then heating to 20° C. and adjusting the mixture of the pH to 7.5 with acetic acid. The mixture is extracted with 5 ml of dichloromethane and the organic phase separated, then washed with 10 ml of water. The solvent was evaporated at a reduced pressure. 274 mg of pantoprazol were obtained (yield: 88%).

후처리

  1. additionwere added
  2. additionwere added
  3. extractionThe mixture is extracted with 5 ml of dichloromethane
  4. customthe organic phase separated
  5. washwashed with 10 ml of water
  6. customThe solvent was evaporated at a reduced pressure

출처 및 근거

ORD 기록
ord-26f0d5e87c4f4edb8c7988c7a56aa63d
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06603009B2

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