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

HRID 2056968

反応式

HRID 2056968 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[CH2:14][C:13]([C:15]([O:17]C)=[O:16])=[C:12]([NH:19][C:20]3[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][CH:21]=3)[CH2:11][C:10]=2[C:27]([O:29]C)=[O:28])=[CH:4][CH:3]=1.[Na].[N+](C1C=C(S(O)(=O)=O)C=CC=1)([O-])=O.[OH-].[Na+].Cl>O.C(O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9]2[CH:14]=[C:13]([C:15]([OH:17])=[O:16])[C:12]([NH:19][C:20]3[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][CH:21]=3)=[CH:11][C:10]=2[C:27]([OH:29])=[O:28])=[CH:6][CH:7]=1

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 73873-Nitrobenzenesulfonic acidHCID 14798Sodium HydroxideHCID 5360545SodiumHCID 147459351,4-Cyclohexadiene-1,4-dicarboxylic acid, 2,5-bis((4-chlorophenyl)amino)-, 1,4-dimethyl ester

生成物 1

HCID 1705571,4-Benzenedicarboxylic acid, 2,5-bis[(4-chlorophenyl)amino]-収率 96%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Dimethyl 2,5-bis{(4-chlorophenyl)amino}cyclohexa-1,4-diene-1,4-dicarboxylate (4.47 gm, 10 mmol), the sodium salt of 3-nitrobenzenesulphonic acid (2.3 gm; 10 mmol), ethanol (70 ml) and 1.0M sodium hydroxide (40 ml) were heated to reflux overnight under a nitrogen atmosphere. The bright yellow solution was allowed to cool and water (120 ml) was added. The mixture was acidified with conc. hydrochloric acid when a red solid precipitated out. This material was filtered off, washed with water and dried under vacuum over phosphorous pentoxide to give 4.0 gm (96%) of 2,5-bis{(4-chlorophenyl)amino}terephthalic acid.

後処理

  1. temperatureto reflux overnight under a nitrogen atmosphere
  2. temperatureto cool
  3. customprecipitated out
  4. filtrationThis material was filtered off
  5. washwashed with water
  6. dry with materialdried under vacuum over phosphorous pentoxide

出典と根拠

ORDレコード
ord-a8c76c812727443dbe2c9b61f7f883bb
出典データセット
uspto-grants-2008_02
特許番号
US07335771B2

関連ノート

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