Methanol → 2-(4,5-dihydro-1H-imidazol-2-yl)benzenethiol

HRID 47284

反応式

HRID 47284 の反応式
[C:1](O)(=O)[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[SH:4].[CH2:11]([NH2:14])[CH2:12][NH2:13].CO>ClC1C=CC=CC=1Cl>[NH:13]1[CH2:12][CH2:11][N:14]=[C:1]1[C:2]1[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=1[SH:4]

参加物

5

反応物 3

HCID 887MethanolHCID 3301EthylenediamineHCID 54432-Mercaptobenzoic Acid

生成物 1

HCID 14773612-(4,5-dihydro-1H-imidazol-2-yl)benzenethiol収率 53.1%

試薬・触媒・溶媒 1

HCID 72391,2-Dichlorobenzene溶媒

反応条件

温度
60 °C

実験手順

To a suspension of 20.0 g (0.112 mol) of thiosalicylic acid in 200 mL of 1,2-dichlorobenzene was added 21.6 mL (0.323 mol) of ethylenediamine. The mixture was refluxed under nitrogen for 4 h then cooled to ca. 60° C. and 50 mL of methanol was added. The solution was allowed to stand at 22° C. over night and the resulting yellow crystalline solid collected and washed with ether to give 10.6 g of pure product.

後処理

  1. temperatureThe mixture was refluxed under nitrogen for 4 h
  2. waitto stand at 22° C. over night
  3. customthe resulting yellow crystalline solid collected
  4. washwashed with ether

出典と根拠

ORDレコード
ord-4a87912f4f5b4b53b7be1e8d5a52c856
出典データセット
uspto-grants-2004_03
特許番号
US06699873B1

関連ノート

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