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

HRID 2262383
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HRID 2262383 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+].O.Cl>CN(C)C=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 962WaterHCID 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 6228Dimethylformamide
용매

실험 절차

The above-prepared 4-methoxy-4′-(di-p-tolylamino)stilbene and twice equimolar amount of sodium ethanethiolate are dissolved in N,N-dimethylformamide, and reacted for 5 hours at 130° C. The mixture is cooled down, and then poured into water and neutralized with hydrochloric acid. The objective material is extracted therefrom using acetic acid. The extracted liquid is washed with water, and then dried. The crude objective material is prepared by removing the solvent (i.e., N,N-dimethylformamide) therefrom. Further, the crude objective material is purified with a column chromatography using silica gel. Thus, 4-hydroxy-4′-(di-p-tolylamino)stilbene (i.e., objective material) is prepared.

후처리

  1. customreacted for 5 hours at 130° C
  2. temperatureThe mixture is cooled down
  3. extractionThe objective material is extracted
  4. washThe extracted liquid is washed with water
  5. customdried
  6. customThe crude objective material is prepared
  7. customby removing the solvent (i.e., N,N-dimethylformamide)
  8. customFurther, the crude objective material is purified with a column chromatography

출처 및 근거

ORD 기록
ord-0091cc6e668d4e369d5e6ef605bc734c
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07851114B2

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