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Dimethylformamide → Sodium 2-[[[5-[[(2,5-dioxo-1-pyrolidinyl)oxy]carbonyl]-2-pyridinyl] hydrazono]methyl]-benzenesulfonate

HRID 1835593
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1835593
[Na+:1].[CH:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10]([O-:13])(=[O:12])=[O:11])=O.N(C1N=CC=CC=1[C:18](O)=[O:19])N.[OH:25][N:26]1[C:30](=[O:31])[CH2:29][CH2:28][C:27]1=[O:32].C1([N:39]=[C:40]=[N:41][CH:42]2[CH2:47][CH2:46][CH2:45]CC2)CCCCC1.C[N:49](C)C=O>CO>[O:32]=[C:27]1[CH2:28][CH2:29][C:30](=[O:31])[N:26]1[O:25][C:18]([C:47]1[CH:46]=[CH:45][C:40]([NH:39][N:49]=[CH:2][C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[S:10]([O-:13])(=[O:12])=[O:11])=[N:41][CH:42]=1)=[O:19].[Na+:1]
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Komponenten

7

Edukt 5

HCID 6228DimethylformamideHCID 10868DicyclohexylcarbodiimideHCID 80170N-HydroxysuccinimideHCID 585323Hydrazinonicotinic acidHCID 3794540Sodium o-formylbenzenesulfonate

Produkt 1

HCID 59642097
Sodium 2-[[[5-[[(2,5-dioxo-1-pyrolidinyl)oxy]carbonyl]-2-pyridinyl] hydrazono]methyl]-benzenesulfonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of 2-formylbenzenesulfonic acid sodium salt (13.6 g) in dimethylformamide (400 mL) was added 2-hydrazinonicotinic acid (10.0 g) and the mixture stirred for three hours. N-hydroxysuccinimide (7.52 g) and dicyclohexylcarbodiimide (27.6 g) were added to the reaction and it was stirred for 16 hours. The mixture was filtered through Celite and the filtrate concentrated under vacuum to a thick oil. This was triturated with ethyl acetate to afford a solid which was filtered to afford crude product (32.8 g). The solids were refluxed in hot methanol for 5 hours, filtered, washed with methanol, and dried under vacuum to afford Sodium 2-[[[5-[[(2,5-dioxo-1-pyrolidinyl)oxy]carbonyl]-2-pyridinyl]hydrazono]methyl]-benzenesulfonate (21.2 g) as a pale yellow solid. NMR (DMSO-d6): 2.88, s (4H); 7.36, m (3H); 7.79, d of d (1H); 8.10, m (2H); 8.79, t (1H); 9.16, s (1H); 11.90, s (1H).

Aufarbeitung

  1. stirringwas stirred for 16 hours
  2. filtrationThe mixture was filtered through Celite
  3. concentrationthe filtrate concentrated under vacuum to a thick oil
  4. customThis was triturated with ethyl acetate
  5. customto afford a solid which
  6. filtrationwas filtered
  7. customto afford crude product (32.8 g)
  8. filtrationfiltered
  9. washwashed with methanol
  10. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-f42379ad136c4988bcd057ce3a80ea21
Quelldatensatz
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06770259B2

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