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

HRID 576480노트

반응식

HRID 576480 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-e429364762db4c338b73196e58fb53c4
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040457B2

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