Acetic Acid → HCID 178488147, 화합물

HRID 492143

반응식

HRID 492143 반응식
[CH3:1][C:2]1[C:3]([CH2:11][S:12][C:13]2[NH:17][C:16]3[CH:18]=[CH:19][C:20]([O:22][CH3:23])=[CH:21][C:15]=3[N:14]=2)=[N:4][CH:5]=[C:6]([CH3:10])[C:7]=1[O:8][CH3:9].[O-:24]S([O-])(=S)=O.[Na+].[Na+].C(O)(=O)C>C(O)C.OO.O>[CH3:10][C:6]1[CH:5]=[N:4][C:3]([CH2:11][S+:12]([O-:24])[C:13]2[NH:17][C:16]3[CH:18]=[CH:19][C:20]([O:22][CH3:23])=[CH:21][C:15]=3[N:14]=2)=[C:2]([CH3:1])[C:7]=1[O:8][CH3:9]

참가 물질

7

반응물 3

HCID 176Acetic AcidHCID 24477Sodium ThiosulfateHCID 178488125HCID 178488125, 화합물

생성물 1

HCID 178488147HCID 178488147, 화합물수율 69%

시약·촉매·용매 3

HCID 702Ethanol용매HCID 784Hydrogen Peroxide용매HCID 962Water용매

실험 절차

0.35 g of 2-[[(3,5-dimethyl-4-methoxy-2-pyridinyl)methyl]thio]-5-methoxy-1H-benzimidazole was suspended in 5 ml of ethanol at room temperature. 0.035 g of Na2WO4·2H2O oxidation catalyst was dissolved in 0.099 g H2O2 (35% aqueous solution), and further diluted with 2 ml of water. The oxidant/catalyst solution was added to the reactant suspension dropwise so that the addition was completed in about 30 minutes while stirring at room temperature. The reaction was continued for additional 6 hours while stirring. 2 ml of 10% Na2S2O3 aqueous solution was then, added, and the resulting mixture was subjected to a reduced pressure to remove ethanol therefrom. Finally, a precipitate was formed after adding a diluted acetic acid aqueous solution to a pH value of about 8, which was filtered, water washed, and dried in vacuo to obtain Omeprazole with a yield of about 69% (LC purity>80%).

후처리

  1. additionThe oxidant/catalyst solution was added to the reactant suspension dropwise so that the addition
  2. waitThe reaction was continued for additional 6 hours
  3. stirringwhile stirring
  4. additionadded
  5. customto remove ethanol
  6. customFinally, a precipitate was formed
  7. filtrationwas filtered
  8. washwater washed
  9. customdried in vacuo

출처 및 근거

ORD 기록
ord-a2a48aa73f364823850070f51b06b7b0
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07531666B2

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