Hydrochloric Acid → 2-Nitro-5-(3-hydroxyphenylthio)-p-xylene

HRID 576480ノート

反応式

HRID 576480 の反応式
[SH:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.[N+:9]([C:12]1[CH:17]=[C:16]([CH3:18])[C:15](Br)=[CH:14][C:13]=1[CH3:20])([O-:11])=[O:10].C([O-])([O-])=O.[K+].[K+].Cl>CN(C)C=O.O>[N+:9]([C:12]1[CH:17]=[C:16]([CH3:18])[C:15]([S:1][C:2]2[CH:7]=[CH:6][CH:5]=[C:4]([OH:8])[CH:3]=2)=[CH:14][C:13]=1[CH3:20])([O-:11])=[O:10]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 8258081-Bromo-2,5-dimethyl-4-nitrobenzeneHCID 27366133-Hydroxybenzenethiol

生成物 1

HCID 665838602-Nitro-5-(3-hydroxyphenylthio)-p-xylene収率 50.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 18.9 g of 3-mercaptophenol (0.150 moles), 32.9 g of 2-nitro-5-bromo-p-xylene (0.143 moles) and K2CO3 (0.143 moles) in 95 ml of N,N-dimethylformamide is stirred at room temperature for 2 hours. A solution of HCl at 10% is added under stirring; the mixture is diluted with H2O and extracted with ethyl acetate. The organic phase is washed again with water, anhydrified on sodium sulfate, filtered and evaporated. 20 g of solid product are obtained, which is used as such for the subsequent reaction.

後処理

  1. stirringunder stirring
  2. extractionextracted with ethyl acetate
  3. washThe organic phase is washed again with water
  4. filtrationfiltered
  5. customevaporated

出典と根拠

ORDレコード
ord-e429364762db4c338b73196e58fb53c4
出典データセット
uspto-grants-2015_05
特許番号
US09040457B2

反応ノート

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