Water → 1,5-bis(4-methoxyphenyl)-3-(methylthio)-1H-1,2,4-triazole

HRID 584733노트

반응식

HRID 584733 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]([SH:22])=[N:10]2)=[CH:5][CH:4]=1.IC.Cl[CH2:26]Cl.O>[OH-].[Na+]>[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][CH3:26])=[N:10]2)=[CH:7][CH:8]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 6344DichloromethaneHCID 178489023HCID 178489023, 화합물

생성물 1

HCID 99234391,5-bis(4-methoxyphenyl)-3-(methylthio)-1H-1,2,4-triazole수율 47.9%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

To a mixture of 1,5-bis(4-methoxyphenyl)-1H-1,2,4-triazole-3-thiol (470 mg, 1.5 mmol) in 1N sodium hydroxide solution (5 mL), was added iodomethane (0.934 mL, 15 mmol). The mixture was shaken overnight. Dichloromethane and water were added to the mixture and the organic layer was separated, washed with 0.1 N hydrochloric acid and sat sodium bicarbonate, and brine, and dried over magnesium sulfate. The solvent was removed under reduced pressure.The generated precipitate was isolated by filtration, washed with diisopropyl ether, and dried in vacuo to give 1,5-bis(4-methoxyphenyl)-3-(methylthio)-1H-1,2,4-triazole (235 mg, 47.9% yield).

후처리

  1. customthe organic layer was separated
  2. washwashed with 0.1 N hydrochloric acid
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customThe generated precipitate was isolated by filtration
  6. washwashed with diisopropyl ether
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-f41dbe4842ff4a748485eb4f21c9d6b5
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06927230B2

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