1,2-Dichloroethane → HCID 22593768, Verbindung

HRID 225859

Reaktionsgleichung

Reaktionsgleichung von HRID 225859
C(Cl)CCl.[NH2:5][C:6]1[N:14]=[CH:13][C:12]([Br:15])=[CH:11][C:7]=1[C:8]([OH:10])=O.[CH2:16]([CH2:18][NH2:19])[OH:17].C1C=CC2N(O)N=NC=2C=1.C(N(C(C)C)CC)(C)C>CN(C=O)C.O>[NH2:5][C:6]1[N:14]=[CH:13][C:12]([Br:15])=[CH:11][C:7]=1[C:8]([NH:19][CH2:18][CH2:16][OH:17])=[O:10]

Komponenten

8

Versuchsvorschrift

EDC (2.91 g, 15.2 mmole) was added to a solution 2-amino-5-bromonicotinic acid (3.00 g, 13.8 mmole), ethanolamine (0.93 g, 15.2 mmole), HOBt.H2O (2.05 g, 15.2 mmole), and diisopropylethylamine (2.64 mL, 15.2 mmole) in DMF (50 mL) at RT and the reaction solution was stirred overnight. The reaction contents were poured into H2O (200 mL) and the resulting mixture was extracted with EtOAc (2×200 mL). The combined organic extracts were washed with H2O and brine and then dried over Na2SO4. Concentration of the organic extracts afforded the tide compound as a yellow solid which was used without further purification: MS (ES) m/e 261 (M+H)+.

Aufarbeitung

  1. customThe reaction contents
  2. extractionthe resulting mixture was extracted with EtOAc (2×200 mL)
  3. washThe combined organic extracts were washed with H2O and brine
  4. dry with materialdried over Na2SO4

Quellen und Nachweise

ORD-Eintrag
ord-8ed8095a5dcd4090ad564ade28f5b802
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07557125B2

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