Potassium Hydroxide → 1,4-Benzenedicarboxylic acid, 2,5-bis[(4-chlorophenyl)amino]-

HRID 399179

반응식

HRID 399179 반응식
C[O:2][C:3](=[O:30])[C:4]1[CH2:13][C:12]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=2)=[C:7]([C:8]([O:10]C)=[O:9])[CH2:6][C:5]=1[NH:22][C:23]1[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][CH:24]=1.[OH-].[K+].[N+](C1C=C(S([O-])(=O)=O)C=CC=1)([O-])=O.[Na+]>C(O)C.O>[Cl:21][C:18]1[CH:19]=[CH:20][C:15]([NH:14][C:12]2[CH:13]=[C:4]([C:3]([OH:30])=[O:2])[C:5]([NH:22][C:23]3[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][CH:24]=3)=[CH:6][C:7]=2[C:8]([OH:10])=[O:9])=[CH:16][CH:17]=1

참가 물질

6

반응물 3

HCID 14797Potassium HydroxideHCID 31389Sodium 3-nitrobenzenesulfonateHCID 147459351,4-Cyclohexadiene-1,4-dicarboxylic acid, 2,5-bis((4-chlorophenyl)amino)-, 1,4-dimethyl ester

생성물 1

HCID 1705571,4-Benzenedicarboxylic acid, 2,5-bis[(4-chlorophenyl)amino]-

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

8.9 Parts of 2,5-di(p-chloroanilino)-3,6-dihydroterephthalic acid dimethyl ester, 50 parts of ethanol, 5.37 parts of KOH, 24.35 parts of water and 6 parts of sodium m-nitrobenzenesulfonate were charged into a 200-ml flask of stainless steel, and refluxed with stirring for 10 hours. When the suspension changed to a black solution, ethanol was steam-distilled, and the reaction mixture was filtered to remove a solid. The remaining solution was heated up to 80° C. with stirring, and after 35 parts of a 10% hydrochloric acid aqueous solution was dropwise added, the mixture was maintained for 1 hour. Then, the mixture was filtered, washed with hot water and dried to give 8.21 parts (98.4% of the theoretical yield) of 2,5-di(p-chloroanilino)terephthalic acid.

후처리

  1. temperaturerefluxed
  2. distillationwas steam-distilled
  3. filtrationthe reaction mixture was filtered
  4. customto remove a solid
  5. stirringwith stirring
  6. additionafter 35 parts of a 10% hydrochloric acid aqueous solution was dropwise added
  7. temperaturethe mixture was maintained for 1 hour
  8. filtrationThen, the mixture was filtered
  9. washwashed with hot water
  10. customdried
  11. customto give 8.21 parts (98.4% of the

출처 및 근거

ORD 기록
ord-c8753250f6fe4010b366681602db5d4c
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05817817

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