Diisopropylethylamine → HCID 69013806, Verbindung

HRID 1371767Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1371767
[NH2:1][CH:2]1[CH2:7][CH2:6][N:5]([S:8]([CH3:11])(=[O:10])=[O:9])[CH2:4][CH:3]1[OH:12].[NH2:13][C:14]1[C:19]([C:20]([C:22]2[C:27]([O:28][CH3:29])=[CH:26][CH:25]=[C:24]([F:30])[C:23]=2[F:31])=[O:21])=[CH:18][N:17]=[C:16](Cl)[N:15]=1.C(N(C(C)C)CC)(C)C>C(O)C>[NH2:13][C:14]1[C:19]([C:20]([C:22]2[C:27]([O:28][CH3:29])=[CH:26][CH:25]=[C:24]([F:30])[C:23]=2[F:31])=[O:21])=[CH:18][N:17]=[C:16]([NH:1][CH:2]2[CH2:7][CH2:6][N:5]([S:8]([CH3:11])(=[O:10])=[O:9])[CH2:4][CH:3]2[OH:12])[N:15]=1

Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 21070550HCID 21070550, VerbindungHCID 21070647HCID 21070647, Verbindung

Produkt 1

HCID 69013806HCID 69013806, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

The amine (44 mg, 0.22 mmol, Example 305) and chloropyrimidine (55 mg, 0.18 mmol, Example 289) were dissolved in ethanol (5 mL). To the stirred mixture at reflux, diisopropylethylamine (64 uL, Aldrich) was added and the mixture was refluxed for 20 hours. The solvent was removed and the residue was purified by HPLC (10–60%, acetonitrile/water) to give a white solid, 25 mg, 30%. MS (ES) MH+=458.

Aufarbeitung

  1. temperatureTo the stirred mixture at reflux
  2. temperaturethe mixture was refluxed for 20 hours
  3. customThe solvent was removed
  4. customthe residue was purified by HPLC (10–60%, acetonitrile/water)
  5. customto give a white solid, 25 mg, 30%

Quellen und Nachweise

ORD-Eintrag
ord-84151c360d744b4ebee4b462e0684f6c
Quelldatensatz
uspto-grants-2007_01
Patentnummer
US07157455B2

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