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

HRID 372224

반응식

HRID 372224 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-6ecf7df2ed454e33b4ecfae66281349c
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04089974

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