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

HRID 584733ノート

反応式

HRID 584733 の反応式
[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

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 6344DichloromethaneHCID 178489023HCID 178489023、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f41dbe4842ff4a748485eb4f21c9d6b5
出典データセット
uspto-grants-2005_08
特許番号
US06927230B2

反応ノート

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