Potassium Carbonate → HCID 178482552, Verbindung

HRID 493698

Reaktionsgleichung

Reaktionsgleichung von HRID 493698
[CH3:1][N:2]1[C:6]([CH3:7])=[C:5]([C:8]([OH:10])=O)[S:4]/[C:3]/1=[N:11]\[CH3:12].[Cl:13][C:14]1[CH:15]=[C:16]2[C:21](=[CH:22][CH:23]=1)[CH:20]=[C:19]([S:24]([CH2:27][CH2:28][C:29]([N:31]1[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]1)=[O:30])(=[O:26])=[O:25])[CH:18]=[CH:17]2.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.C(=O)([O-])[O-].[K+].[K+]>ClCCl.C(N(CC)CC)C>[Cl:13][C:14]1[CH:15]=[C:16]2[C:21](=[CH:22][CH:23]=1)[CH:20]=[C:19]([S:24]([CH2:27][CH2:28][C:29]([N:31]1[CH2:32][CH2:33][N:34]([C:8]([C:5]3[S:4]/[C:3](=[N:11]\[CH3:12])/[N:2]([CH3:1])[C:6]=3[CH3:7])=[O:10])[CH2:35][CH2:36]1)=[O:30])(=[O:26])=[O:25])[CH:18]=[CH:17]2

Komponenten

8

Edukt 5

HCID 11430Potassium CarbonateHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 231308831-(3-((6-Chloro-2-naphthyl)sulfonyl)propionyl)piperazineHCID 178482553HCID 178482553, Verbindung

Produkt 1

HCID 178482552HCID 178482552, VerbindungAusbeute 8,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

(2Z)-3,4-Dimethyl-2-methylimino-2,3-dihydro-1,3-thiazole-5-carboxylic acid (0.6 g) was dissolved in dichloromethane (30 mL), and triethylamine (0.14 mL) was added thereto. With ice cooling, 1-(3-((6-chloro-2-naphthyl)sulfonyl)propionyl)piperazine (1.0 g), HOBt (0.42 g) and WSC (0.57 g) were added thereto, and the mixture was mixed at room temperature for 16 hours. The reaction solution was basified with an aqueous potassium carbonate solution, then extracted with chloroform, and the extract was dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified with a basic silica gel column to give the title compound (0.13 g) as a white powder.

Aufarbeitung

  1. additionthe mixture was mixed at room temperature for 16 hours
  2. extractionextracted with chloroform
  3. dry with materialthe extract was dried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off
  5. customthe residue was purified with a basic silica gel column

Quellen und Nachweise

ORD-Eintrag
ord-c46f2e1a308a4935b48dc3efa5d19905
Quelldatensatz
uspto-grants-2009_05
Patentnummer
US07534887B2

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