Acetic Acid → HCID 178488147, 화합물

HRID 492137

반응식

HRID 492137 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].[OH-].[Na+].[O-:26]S([O-])(=S)=O.[Na+].[Na+].C(O)(=O)C>CO.O.OO>[CH3:10][C:6]1[CH:5]=[N:4][C:3]([CH2:11][S+:12]([O-:26])[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

8

반응물 4

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 24477Sodium ThiosulfateHCID 178488125HCID 178488125, 화합물

생성물 1

HCID 178488147HCID 178488147, 화합물수율 88%

시약·촉매·용매 3

HCID 784Hydrogen Peroxide용매HCID 887Methanol용매HCID 962Water용매2회

실험 절차

2 g of 2-[[(3,5-dimethyl-4-methoxy-2-pyridinyl)methyl]thio]-5-methoxy-1H-benzimidazole was suspended in 36 ml of methanol at room temperature, to which 1.88 g of 45% NaOH in 14 ml water was added while stirring. 0.09 g of Na2WO4·2H2O oxidation catalyst was dissolved in 0.74 g H2O2 (50% aqueous solution), and further diluted with 10 ml. of water. The oxidant/catalyst solution was added to the reactant/base solution dropwise so that the addition was completed in about 30 minutes while stirring at room temperature. The reaction was continued for additional 10 minutes while stirring. 10 ml of 10% Na2S2O3 aqueous solution was then added, and the resulting mixture was subjected to a reduced pressure to remove methanol 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 88% (LC purity>95%).

후처리

  1. additionwas added
  2. additionfurther diluted with 10 ml
  3. additionThe oxidant/catalyst solution was added to the reactant/base solution dropwise so that the addition
  4. stirringwhile stirring at room temperature
  5. waitThe reaction was continued for additional 10 minutes
  6. stirringwhile stirring
  7. customto remove methanol
  8. customFinally, a precipitate was formed
  9. filtrationwas filtered
  10. washwater washed
  11. customdried in vacuo

출처 및 근거

ORD 기록
ord-64e677ad853640a1a3b4e16b56b62177
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07531666B2

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