Sodium Carbonate → 4,4'-[5-Carboxy-1,3-phenylenebis(carbonylimino)]-diphthalic acid pentasodium salt

HRID 372224

反応式

HRID 372224 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([C:11]([OH:13])=[O:12])[C:5](=[CH:9][CH:10]=1)[C:6]([OH:8])=[O:7].[OH-:14].[Na+:15].[C:16](=[O:19])([O-:18])[O-].[Na+].[Na+].[C:22]1([C:34](Cl)=[O:35])[CH:27]=[C:26]([C:28](Cl)=[O:29])[CH:25]=[C:24]([C:31](Cl)=[O:32])[CH:23]=1>O>[Na+:15].[Na+:15].[Na+:15].[Na+:15].[Na+:15].[C:34]([C:22]1[CH:27]=[C:26]([C:28]([NH:1][C:2]2[CH:3]=[C:4]([C:11]([O-:13])=[O:12])[C:5](=[CH:9][CH:10]=2)[C:16]([O-:18])=[O:19])=[O:29])[CH:25]=[C:24]([C:31]([NH:1][C:2]2[CH:3]=[C:4]([C:11]([O-:13])=[O:12])[C:5](=[CH:9][CH:10]=2)[C:6]([O-:8])=[O:7])=[O:32])[CH:23]=1)([OH:35])=[O:14]

参加物

6

反応物 4

HCID 10340Sodium CarbonateHCID 14798Sodium HydroxideHCID 729124-Aminophthalic acidHCID 78138Trimesoyl chloride

生成物 1

HCID 1371959144,4'-[5-Carboxy-1,3-phenylenebis(carbonylimino)]-diphthalic acid pentasodium salt

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A 2.5 g portion of 4-amino phthalic acid stirred in 100 ml of water is neutralized to pH 7.2 with sodium hydroxide then 1.47 g of sodium carbonate is added. To this solution is added dropwise 1.21 g of 1,3,5-benzenetricarboxylic acid chloride with vigorous stirring. Stirring is continued for 18 hours, then the reaction mixture is concentrated, dissolved in 60 ml of water and acidified with hydrochloric acid. The precipitate is filtered and washed with ethanol and ether to yield 2.8 g of product. This product is dissolved in 50 ml of water, is neutralized and fractionally precipitated with ethanol 6 times. The final crop, 523 mg, is identified as the product of the Example.

後処理

  1. concentrationthe reaction mixture is concentrated
  2. dissolutiondissolved in 60 ml of water
  3. filtrationThe precipitate is filtered
  4. washwashed with ethanol and ether

出典と根拠

ORDレコード
ord-6ecf7df2ed454e33b4ecfae66281349c
出典データセット
uspto-grants-1978_05
特許番号
US04089974

関連ノート

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