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Hydrochloric Acid → 2-(4-Methylthiobenzyl)amino-5-fluoronitrobenzene

HRID 893361
ノート
印刷プレビュー

反応式

HRID 893361 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[N+:9]([O-:11])=[O:10].[CH3:12][S:13][C:14]1[CH:21]=[CH:20][C:17]([CH2:18]Cl)=[CH:16][CH:15]=1.C([O-])(=O)C.[Na+].Cl>II>[CH3:12][S:13][C:14]1[CH:21]=[CH:20][C:17]([CH2:18][NH:1][C:2]2[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=2[N+:9]([O-:11])=[O:10])=[CH:16][CH:15]=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 313Hydrochloric AcidHCID 677694-Fluoro-2-nitroanilineHCID 701281-(Chloromethyl)-4-(methylthio)benzeneHCID 517045Sodium Acetate

生成物 1

HCID 149529802-(4-Methylthiobenzyl)amino-5-fluoronitrobenzene収率 51.3%

試薬・触媒・溶媒 1

HCID 807Iodine
触媒

反応条件

温度
120 °C

実験手順

24.8 g of 2-amino-5-fluoronitrobenzene and 27.6 g of 4-methylthiobenzyl chloride are mixed and 14.4 g of anhydrous sodium acetate and 0.3 g of iodine are added. The mixture is heated at 120° C. for 12 hours, with stirring, and is then cooled, taken up with a dilute solution of hydrochloric acid and extracted with ethyl acetate. The organic phase is washed with dilute hydrochloric acid and then with water, dried over magnesium sulfate and evaporated to dryness. The oil obtained crystallizes from isopropyl ether to give 23.8 g of 2-(4-methylthiobenzyl)amino-5-fluoronitrobenzene in the form of crystals melting at 117° C.

後処理

  1. temperatureis then cooled
  2. extractionextracted with ethyl acetate
  3. washThe organic phase is washed with dilute hydrochloric acid
  4. dry with materialwith water, dried over magnesium sulfate
  5. customevaporated to dryness
  6. customThe oil obtained
  7. customcrystallizes from isopropyl ether

出典と根拠

ORDレコード
ord-0bee4deba4e348efbd8919a1992f907b
出典データセット
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05124336

反応ノート

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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