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

HRID 2096101
ノート
印刷プレビュー

反応式

HRID 2096101 の反応式
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
参加物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 6228DimethylformamideHCID 4459711Sodium ethanethiolateHCID 538532054-[2-(4-Methoxyphenyl)ethenyl]-N,N-bis(4-methylphenyl)aniline

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8d5304243bcd4ebb8a615f1ac18b9557
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08450033B2

反応ノート

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