3-Nitrobenzenesulfonyl chloride → 8-m-Nitrobenzenesulfonamido-1,3,6-naphthalenetrisulfonic acid

HRID 224338

반응식

HRID 224338 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([S:20]([OH:23])(=[O:22])=[O:21])[CH:5]=[C:6]2[C:11]=1[C:10]([S:12]([OH:15])(=[O:14])=[O:13])=[CH:9][C:8]([S:16]([OH:19])(=[O:18])=[O:17])=[CH:7]2.C1C(N=NC2C(=O)N(C3C=CC(S([O-])(=O)=O)=CC=3)N=C2C([O-])=O)=CC=C(S([O-])(=O)=O)C=1.[Na+].[Na+].[Na+].C(=O)([O-])[O-].[Na+].[Na+].[N+:64]([C:67]1[CH:68]=[C:69]([S:73](Cl)(=[O:75])=[O:74])[CH:70]=[CH:71][CH:72]=1)([O-:66])=[O:65]>O>[N+:64]([C:67]1[CH:68]=[C:69]([S:73]([NH:1][C:2]2[CH:3]=[C:4]([S:20]([OH:23])(=[O:22])=[O:21])[CH:5]=[C:6]3[C:11]=2[C:10]([S:12]([OH:15])(=[O:14])=[O:13])=[CH:9][C:8]([S:16]([OH:19])(=[O:17])=[O:18])=[CH:7]3)(=[O:75])=[O:74])[CH:70]=[CH:71][CH:72]=1)([O-:66])=[O:65]

참가 물질

6

반응물 4

HCID 84763-Nitrobenzenesulfonyl chloride2회HCID 10340Sodium Carbonate2회HCID 649518-Aminonaphthalene-1,3,6-trisulfonic acidHCID 164825Tartrazine

생성물 1

HCID 131521328-m-Nitrobenzenesulfonamido-1,3,6-naphthalenetrisulfonic acid수율 80.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred solution of 21.9 g of 8-amino-1,3,6-naphthalenetrisulfonic acid, trisodium salt and 11.4 g of anhydrous sodium carbonate in 280 ml of water is added 24.0 g of m-nitrobenzenesulfonyl chloride. The mixture is stirred at room temperature for 16 hours, then an additional 1.0 g of sodium carbonate and 2.0 g of m-nitrobenzenesulfonyl chloride are added and stirring is continued for 3 hours longer. The mixture is evaporated and the residue is dissolved in 200 ml of water. A copious amount of absolute ethanol is added and the solid formed is collected and washed with ethanol and ether, then is dried to yield 26.1 g of 8-m-nitrobenzenesulfonamido-1,3,6-naphthalenetrisulfonic acid, trisodium salt.

후처리

  1. stirringstirring
  2. waitis continued for 3 hours
  3. customThe mixture is evaporated
  4. dissolutionthe residue is dissolved in 200 ml of water
  5. additionA copious amount of absolute ethanol is added
  6. customthe solid formed
  7. customis collected
  8. washwashed with ethanol and ether
  9. customis dried

출처 및 근거

ORD 기록
ord-9fce3d7684704acea5ef02fcfaa688f6
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04231958

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