Sodium Acetate → HCID 178496248, Verbindung

HRID 339166

Reaktionsgleichung

Reaktionsgleichung von HRID 339166
[C:1]([CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][N+:9]1[C:17]2[C:12](=[CH:13][C:14]([S:18]([OH:21])(=[O:20])=[O:19])=[CH:15][CH:16]=2)[C:11]([CH3:29])([CH2:22][CH2:23][CH2:24][S:25]([OH:28])(=[O:27])=[O:26])[C:10]=1/[CH:30]=[CH:31]/NC1C=CC=CC=1)([OH:3])=[O:2].[CH3:39][O:40][CH2:41][CH2:42][O:43][CH2:44][CH2:45][O:46][CH2:47][CH2:48][N+:49]1[C:57]2[C:52](=[CH:53][C:54]([S:58]([OH:61])(=[O:60])=[O:59])=[CH:55][CH:56]=2)[C:51]([CH3:69])([CH2:62][CH2:63][CH2:64][S:65]([OH:68])(=[O:67])=[O:66])[C:50]=1[CH3:70].C([O-])(=O)C.[Na+:75].COCCOCC[N+]1C2C(=CC(S(O)(=O)=O)=CC=2)C(C)(CCCS(O)(=O)=O)C=1C>C(O)(=O)C.C(OC(=O)C)(=O)C.C(OCC)C>[Na+:75].[Na+:75].[Na+:75].[C:1]([CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][N:9]1[C:17]2[C:12](=[CH:13][C:14]([S:18]([OH:21])(=[O:20])=[O:19])=[CH:15][CH:16]=2)[C:11]([CH3:29])([CH2:22][CH2:23][CH2:24][S:25]([OH:28])(=[O:26])=[O:27])/[C:10]/1=[CH:30]\[CH:31]=[CH:70]\[C:50]1[C:51]([CH3:69])([CH2:62][CH2:63][CH2:64][S:65]([OH:68])(=[O:67])=[O:66])[C:52]2[C:57](=[CH:56][CH:55]=[C:54]([S:58]([OH:61])(=[O:59])=[O:60])[CH:53]=2)[N+:49]=1[CH2:48][CH2:47][O:46][CH2:45][CH2:44][O:43][CH2:42][CH2:41][O:40][CH3:39])([OH:3])=[O:2]

Komponenten

7

Edukt 4

HCID 517045Sodium AcetateHCID 885363471-(5-carboxypentyl)-3-methyl-2-((E)-2-phenylamino-vinyl)-5-sulfo-3-(3-sulfopropyl)-3H-indoliumHCID 885363611-[2-(2-methoxy-ethoxy)-ethyl]-2,3-dimethyl-5-sulfo-3-(3-sulfopropyl)-3H-indolium2×HCID 885363881-{2-[2-(2-methoxy-ethoxy)-ethoxy]-ethyl}-2,3-dimethyl-5-sulfo-3-(3-sulfo-propyl)-3H-indolium

Produkt 1

HCID 178496248HCID 178496248, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 21895370AcOH AcOAcLösungsmittel

Versuchsvorschrift

One mmol 1-(5-carboxypentyl)-3-methyl-2-((E)-2-phenylamino-vinyl)-5-sulfo-3-(3-sulfopropyl)-3H-indolium and 1 mmol 1-{2-[2-(2-methoxy-ethoxy)-ethoxy]-ethyl}-2,3-dimethyl-5-sulfo-3-(3-sulfo-propyl)-3H-indolium were dissolved in 20 ml acetic acid/acetic anhydride (1/1) followed by the addition of 200 mg sodium acetate. The solution was stirred under reflux for 15 min. After cooling to room temperature, 20 ml diethylether was added. The resulting precipitate (mixture of the diastereomers 550-1 compound 2 and 550-2 compound 2) was extracted by suction, washed with ether and dried.

Aufarbeitung

  1. temperatureunder reflux for 15 min
  2. extractionwas extracted by suction
  3. washwashed with ether
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-e9a60811a3444b65937bea7780beb8aa
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08889884B1

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