Diisopropylethylamine → HCID 178431856, Verbindung

HRID 1429801Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1429801
Cl.[NH2:2][CH:3]([C:5]1[N:6]=[C:7]2[S:22][CH:21]=[C:20]([CH3:23])[N:8]2[C:9](=[O:19])[C:10]=1[C:11]1[CH:16]=[C:15]([F:17])[CH:14]=[C:13]([F:18])[CH:12]=1)[CH3:4].[F:24][C:25]1[N:33]=[C:32]2[C:28]([NH:29][CH:30]=[N:31]2)=[C:27](Cl)[N:26]=1.C(N(CC)C(C)C)(C)C>C(O)(C)C>[F:18][C:13]1[CH:12]=[C:11]([C:10]2[C:9](=[O:19])[N:8]3[C:20]([CH3:23])=[CH:21][S:22][C:7]3=[N:6][C:5]=2[CH:3]([NH:2][C:27]2[N:26]=[C:25]([F:24])[N:33]=[C:32]3[C:28]=2[N:29]=[CH:30][NH:31]3)[CH3:4])[CH:16]=[C:15]([F:17])[CH:14]=1

Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 52879146-Chloro-2-fluoropurineHCID 668644077-(1-aminoethyl)-6-(3,5-difluorophenyl)-3-methyl-5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one hydrochloride

Produkt 1

HCID 178431856HCID 178431856, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 7-(1-aminoethyl)-6-(3,5-difluorophenyl)-3-methyl-5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one hydrochloride (0.030 g, 0.084 mmol), 2-fluoro-6-chloropurine (0.015 g, 0.084 mmol), and N,N-diisopropylethylamine (0.044 mL, 0.25 mmol) in isopropyl alcohol (0.2 mL) was heated at 100° C. for three days, in a sealed tube. The resultant mixture was purified on RP-HPLC (XBridge C18 Column, eluting with a gradient of acetonitrile/water containing 0.15% NH4OH) to give the desired product. LCMS calculated for C20H15F3N7OS (M+H)+: m/z=458.1. Found: 458.0.

Aufarbeitung

  1. customThe resultant mixture was purified on RP-HPLC (XBridge C18 Column
  2. washeluting with a gradient of acetonitrile/water containing 0.15% NH4OH)

Quellen und Nachweise

ORD-Eintrag
ord-e2f38595212a4d21bfc05e9b806fd9b6
Quelldatensatz
uspto-grants-2015_01
Patentnummer
US08940752B2

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