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1,2-Dichlorobenzene → 3-(2-chlorophenyl)-1-methyl-5-[4-(6-methylhexyl)phenyl]-1H-1,2,4-triazole

HRID 1108946
ノート
印刷プレビュー

反応式

HRID 1108946 の反応式
[CH3:1][N:2](S(C1C=CC=CC=1)(=O)=O)[N:3]=[C:4](Cl)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[Cl:11].[CH3:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][C:29]1[CH:36]=[CH:35][C:32]([C:33]#[N:34])=[CH:31][CH:30]=1.[Cl-].[Al+3].[Cl-].[Cl-].ClC1C=CC=CC=1Cl>C(Cl)(Cl)Cl>[Cl:11][C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=1[C:4]1[N:34]=[C:33]([C:32]2[CH:35]=[CH:36][C:29]([CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH3:22])=[CH:30][CH:31]=2)[N:2]([CH3:1])[N:3]=1
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 5758634-HeptylbenzonitrileHCID 6451240Aluminum(III) ChlorideHCID 54508988N-methyl-N-phenylsulfonyl-2-chlorobenzohydrazonoyl chloride

生成物 1

HCID 190213703-(2-chlorophenyl)-1-methyl-5-[4-(6-methylhexyl)phenyl]-1H-1,2,4-triazole収率 68.8%

試薬・触媒・溶媒 1

HCID 6212
Chloroform
溶媒

反応条件

温度
140 °C

実験手順

A mixture of 2.06 g of N-methyl-N-phenylsulfonyl-2-chlorobenzohydrazonoyl chloride, 1.30 g of 4-(6-methylhexyl) benzonitrile, 0.93 g of anhydrous aluminum chloride and 5 ml of o-dichlorobenzene was stirred in an oil bath at a temperature of 140° C. for 30 minutes. After the cooling, the resulting solution was dissolved in 200 ml of chloroform, washed with diluted hydrochloric acid solution, diluted sodium hydroxide aqueous solution and saline water in this order, dried over anhydrous magnesium sulfate and concentrated under a reduced pressure. The resulting concentrate was purified through a chromatography of silica gel column using a mixed solution of hexane and ethyl acetate as a developing solvent to obtain 1.52 g of the given compound (melting point: 64.0°-67.0° C.).

後処理

  1. washwashed with diluted hydrochloric acid solution, diluted sodium hydroxide aqueous solution and saline water in this order
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated under a reduced pressure
  4. concentrationThe resulting concentrate
  5. customwas purified through a chromatography of silica gel column

出典と根拠

ORDレコード
ord-22797ca54e3d48d7b448cc4eef35e9f1
出典データセット
uspto-grants-1994_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05318959

反応ノート

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