m-Chloroperbenzoic acid → 1,5-bis(4-methoxyphenyl)-3-(methylsulfonyl)-1H-1,2,4-triazole

HRID 584735노트

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HRID 584735 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:13]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=3)=[N:12][C:11]([S:22]([CH3:24])=[O:23])=[N:10]2)=[CH:5][CH:4]=1.ClC1C=CC=C(C(OO)=[O:33])C=1.C(=O)(O)[O-].[Na+]>ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([N:9]2[C:13]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=3)=[N:12][C:11]([S:22]([CH3:24])(=[O:33])=[O:23])=[N:10]2)=[CH:7][CH:8]=1

참가 물질

5

반응물 3

HCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 102689921,5-bis(4-methoxyphenyl)-3-(methylsulfinyl)-1H-1,2,4-triazole

생성물 1

HCID 99687881,5-bis(4-methoxyphenyl)-3-(methylsulfonyl)-1H-1,2,4-triazole수율 81.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A mixture of 1,5-bis(4-methoxyphenyl)-3-(methylsulfinyl)-1H-1,2,4-triazole (152 mg, 0.443 mmol) and m-chloroperbenzoic acid (115 mg, 0.664 mmol) in dichloromethane (1.5 mL) was stirred at room temperature for 6 hours. Dichloromethane and sat. sodium bicarbonate solution were poured into the mixture and the organic layer was separated. The aqueous layer was extracted with dichloromethane. A combined organic layer was washed with sat. sodium bicarbonate solution and brine and dried over magnesium sulfate. The solvent was removed under reduced pressure. The residue was triturated with diisopropyl ether and the precipitate was isolated by filtration, washed with diisopropyl ether, and dried in vacuo to give 1,5-bis(4-methoxyphenyl)-3-(methylsulfonyl)-1H-1,2,4-triazole (130 mg, 81.7% yield).

후처리

  1. customthe organic layer was separated
  2. extractionThe aqueous layer was extracted with dichloromethane
  3. washA combined organic layer was washed with sat. sodium bicarbonate solution and brine
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customThe residue was triturated with diisopropyl ether
  7. customthe precipitate was isolated by filtration
  8. washwashed with diisopropyl ether
  9. customdried in vacuo

출처 및 근거

ORD 기록
ord-14d159d1008045edbab71a28d3c1cd2b
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06927230B2

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