Acetic Acid → HCID 178495390, 화합물

HRID 394826노트

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HRID 394826 반응식
[CH3:1][C:2]1[C:3]([CH2:14][S:15][C:16]2[NH:20][C:19]3[CH:21]=[CH:22][CH:23]=[CH:24][C:18]=3[N:17]=2)=[N:4][CH:5]=[CH:6][C:7]=1[O:8][CH2:9][CH2:10][CH2:11][O:12][CH3:13].C([O-])([O-])=[O:26].C([O-])([O-])=O.OO.OO.OO.[Na+].[Na+].[Na+].[Na+].O.C(O)(=O)C>CO.[NH4+].[NH4+].[O-][Mo]([O-])(=O)=O>[CH3:1][C:2]1[C:3]([CH2:14][S+:15]([O-:26])[C:16]2[NH:20][C:19]3[CH:21]=[CH:22][CH:23]=[CH:24][C:18]=3[N:17]=2)=[N:4][CH:5]=[CH:6][C:7]=1[O:8][CH2:9][CH2:10][CH2:11][O:12][CH3:13]

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 159762Sodium percarbonateHCID 9949996Rabeprazole-thioether

생성물 1

HCID 178495390HCID 178495390, 화합물수율 200.8%

시약·촉매·용매 2

HCID 61578Diammonium molybdate촉매HCID 887Methanol용매

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온도
5 °C

실험 절차

2.3 g of 2-[[[3-methyl-4-(3-methoxypropoxy)-2-pyridinyl]methyl]thio]-1H-benzimidazol were dissolved in 11.5 ml of methanol and 90 mg of ammonium molybdate were added. The solution was cooled to 5° C. and 0.87 g of sodium percarbonate were added, then kept stirred at this temperature for 6 h. After the reaction finished 22 ml of water were added, then heating to 20° C. and adjusting the pH of the mixture to 7.5 with acetic acid. The mixture is extracted with 50 ml of dichloromethane and the organic phase was separated, which was then washed with 100 ml of water. The solvent was evaporated at a reduced pressure. 2.0 g of rabeprazol were obtained (yield: 81%).

후처리

  1. additionwere added
  2. temperatureheating to 20° C.
  3. extractionThe mixture is extracted with 50 ml of dichloromethane
  4. customthe organic phase was separated
  5. washwhich was then washed with 100 ml of water
  6. customThe solvent was evaporated at a reduced pressure

출처 및 근거

ORD 기록
ord-829b935ad71c4a469b1fe5253629418b
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06603009B2

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