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1,2-Dichlorobenzene → 5-(4-t-butyl-2-ethoxyphenyl)-3-(2-chloro-6-fluorophenyl) 1-methyl-1H-1,2,4-triazole

HRID 52208
ノート
印刷プレビュー

反応式

HRID 52208 の反応式
[CH3:1][N:2](S(C1C=CC=CC=1)(=O)=O)[N:3]=[C:4](Cl)[C:5]1[C:10]([F:11])=[CH:9][CH:8]=[CH:7][C:6]=1[Cl:12].[C:23]([C:27]1[CH:34]=[CH:33][C:30]([C:31]#[N:32])=[C:29]([O:35][CH2:36][CH3:37])[CH:28]=1)([CH3:26])([CH3:25])[CH3:24].[Cl-].[Al+3].[Cl-].[Cl-].ClC1C=CC=CC=1Cl>C(Cl)(Cl)Cl>[C:23]([C:27]1[CH:34]=[CH:33][C:30]([C:31]2[N:2]([CH3:1])[N:3]=[C:4]([C:5]3[C:10]([F:11])=[CH:9][CH:8]=[CH:7][C:6]=3[Cl:12])[N:32]=2)=[C:29]([O:35][CH2:36][CH3:37])[CH:28]=1)([CH3:26])([CH3:24])[CH3:25]
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 4

HCID 72391,2-DichlorobenzeneHCID 6451240Aluminum(III) ChlorideHCID 214636124-(tert-Butyl)-2-ethoxybenzonitrileHCID 53760501N-methyl-N-phenylsulfonyl-2-chloro-6-fluorobenzohydrazonoyl chloride

生成物 1

HCID 214636525-(4-t-butyl-2-ethoxyphenyl)-3-(2-chloro-6-fluorophenyl) 1-methyl-1H-1,2,4-triazole収率 11.6%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
140 °C

実験手順

A mixture of N-methyl-N-(benzenesulfonyl)-2-chloro-6-fluorobenzohydrazonoyl chloride (1.60 g), 4-t-butyl-2-ethoxybenzonitrile (1.00 g), anhydrous aluminum chloride (0.60 g) and o-dichlorobenzene (5 ml) is stirred at an oil bath temperature of 140° C. for 30 minutes. After cooling, the reaction mixture is dissolved in chloroform (100 ml), washed with dilute hydrochloric acid, dilute aqueous solution of sodium hydroxide and saline in this order, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The concentrate is purified by silica gel column chromatography using mixed solvent of hexane-ethyl acetate as eluent to give 0.20 g of desired compound (melting point: 108.0°-111.0° C.).

後処理

  1. temperatureAfter cooling
  2. washwashed with dilute hydrochloric acid, dilute aqueous solution of sodium hydroxide and saline in this order
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe concentrate is purified by silica gel column chromatography
  6. additionusing mixed solvent of hexane-ethyl acetate as eluent

出典と根拠

ORDレコード
ord-6b89963f43084c7982e0894815771522
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05616594

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