Acetic Acid → Lansoprazole

HRID 394825

반응식

HRID 394825 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][C:10]([F:13])([F:12])[F:11].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:7]([O:8][CH2:9][C:10]([F:12])([F:11])[F:13])=[CH:6][CH:5]=[N:4][C:3]=1[CH2:14][S+:15]([O-:26])[C:16]1[NH:20][C:19]2[CH:21]=[CH:22][CH:23]=[CH:24][C:18]=2[N:17]=1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 159762Sodium percarbonateHCID 1094080Lansoprazole sulfide

생성물 1

HCID 3883Lansoprazole수율 238.6%

시약·촉매·용매 2

HCID 61578Diammonium molybdate촉매HCID 887Methanol용매

반응 조건

온도
10 °C

실험 절차

10 g of 2-[[[3-methyl-4-(2,2,2-trifluoroethoxy)-2-pyridinyl]methyl]thio]-1H-benzimidazol were dissolved in 50 ml of methanol and 0.3 g of ammonium molybdate were added. The solution was cooled to 10° C., and 3.35 g of sodium percarbonate added slowly, kept stirred at the same temperature for 15 hours. After the reaction ended 250 ml of water were added and the pH of the resulting mixture adjusted to 10 with 10% acetic acid. This was kept stirred for 1 hour and the solid obtained was filtered, and subsequently washed with water and dried in a vacuum oven at 40° C. This provided 9.4 g of lansoprazol (yield: 90%).

후처리

  1. additionwere added
  2. stirringThis was kept stirred for 1 hour
  3. customthe solid obtained
  4. filtrationwas filtered
  5. washsubsequently washed with water
  6. customdried in a vacuum oven at 40° C

출처 및 근거

ORD 기록
ord-858f083ce39e4c66a135dc371a8ec34e
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06603009B2

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