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1H-1,2,4-Triazole → HCID 15433416、化合物

HRID 613394
ノート
印刷プレビュー

反応式

HRID 613394 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1([O:19][CH2:18]1)[C:10]([F:17])([F:16])[S:11][CH2:12][CH2:13][O:14][CH3:15].[NH:20]1[CH:24]=[N:23][CH:22]=[N:21]1.C(=O)([O-])[O-].[K+].[K+]>CS(C)=O.CCOCC>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:19])([CH2:18][N:20]1[CH:24]=[N:23][CH:22]=[N:21]1)[C:10]([F:17])([F:16])[S:11][CH2:12][CH2:13][O:14][CH3:15]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 154343832-(2,4-Difluorophenyl)-1,1-difluoro-1-(2-methoxyethyl)thio-2,3-epoxypropane

生成物 1

HCID 15433416HCID 15433416、化合物収率 12.4%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 3283
Diethyl Ether
溶媒

反応条件

温度
50 °C

実験手順

To a solution of 2-(2,4-difluorophenyl)-1,1-difluoro-1-[(2-methoxyethyl)thio]-2,3-epoxypropane (13.0 g, 0.044 mol) in DMSO (100 ml), 1,2,4-triazole (7.6 g, 0.11 mol) and potassium carbonate (15.2 g, 0.11 mol) were added and the resulting mixture was stirred at room temperature for 12 hours and at an external temperature of 50° C. for one hour. After the completion of the reaction, the reaction mixture was diluted with ether and insoluble matter was filtered off. The ether solution was washed with water, dried over magnesium sulfate and distilled off under reduced pressure. The residue was recrystallized from isopropyl ether-ethyl acetate, whereby 2-(2,4-difluorophenyl)-1,1-difluoro-1-[(2-methoxyethyl)thio]-3-(1H-1,2,4-triazol-1-yl)-2-propanol (2.0 g, yield: 12.0%) was obtained as colorless crystals.

後処理

  1. customAfter the completion of the reaction
  2. filtrationwas filtered off
  3. washThe ether solution was washed with water
  4. dry with materialdried over magnesium sulfate
  5. distillationdistilled off under reduced pressure
  6. customThe residue was recrystallized from isopropyl ether-ethyl acetate

出典と根拠

ORDレコード
ord-15fd9a3188044b8b8f147b93b4373b2a
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06008239

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート