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Hydrochloric Acid → 4-(2-{4-[Bis(4-methylphenyl)amino]phenyl}ethenyl)phenol

HRID 2096101
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HRID 2096101 반응식
C[O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]=[CH:10][C:11]2[CH:16]=[CH:15][C:14]([N:17]([C:25]3[CH:30]=[CH:29][C:28]([CH3:31])=[CH:27][CH:26]=3)[C:18]3[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][CH:19]=3)=[CH:13][CH:12]=2)=[CH:5][CH:4]=1.C([S-])C.[Na+].CN(C)C=O.Cl>O>[OH:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]=[CH:10][C:11]2[CH:16]=[CH:15][C:14]([N:17]([C:25]3[CH:26]=[CH:27][C:28]([CH3:31])=[CH:29][CH:30]=3)[C:18]3[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][CH:19]=3)=[CH:13][CH:12]=2)=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 4459711Sodium ethanethiolateHCID 538532054-[2-(4-Methoxyphenyl)ethenyl]-N,N-bis(4-methylphenyl)aniline

생성물 1

HCID 599226714-(2-{4-[Bis(4-methylphenyl)amino]phenyl}ethenyl)phenol

시약·촉매·용매 1

HCID 962
Water
용매

실험 절차

The obtained 4-methoxy-4′-(di-p-tolylamino)stilbene and two equivalent amounts of sodium ethanethiolate were dissolved into N,N-dimethylformamide, allowing reaction to proceed at 130° C. for 5 hours. The solution was cooled, added in water, and neutralized with hydrochloric acid, and the target product was extracted with ethyl acetate. The extract liquid was washed with water and dried, and solvent was removed to obtain a crude product, which was then purified by column chromatography on silica gel to give 4-hydroxy-4′-(di-p-tolylamino)stilbene (CTP-1), a target product.

후처리

  1. customreaction
  2. temperatureThe solution was cooled
  3. extractionthe target product was extracted with ethyl acetate
  4. washThe extract liquid was washed with water
  5. customdried
  6. customsolvent was removed
  7. customto obtain a crude product, which
  8. customwas then purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-8d5304243bcd4ebb8a615f1ac18b9557
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08450033B2

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