Thiocarbonyl diimidazole → HCID 59857446, Verbindung

HRID 555416Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 555416
[C:1]([C:5]1[CH:20]=[CH:19][CH:18]=[CH:17][C:6]=1[O:7][C:8]1[N:13]=[C:12]([NH:14][CH3:15])[CH:11]=[CH:10][C:9]=1[NH2:16])([CH3:4])([CH3:3])[CH3:2].[C:21](C1NC=CN=1)(C1NC=CN=1)=[S:22]>C(Cl)Cl>[C:1]([C:5]1[CH:20]=[CH:19][CH:18]=[CH:17][C:6]=1[O:7][C:8]1[N:13]=[C:12]([NH:14][CH3:15])[CH:11]=[CH:10][C:9]=1[N:16]=[C:21]=[S:22])([CH3:4])([CH3:2])[CH3:3]

Komponenten

4

Edukt 2

HCID 11412697Thiocarbonyl diimidazoleHCID 598573486-(2-tert-Butylphenoxy)-N2-methylpyridine-2,5-diamine

Produkt 1

HCID 59857446HCID 59857446, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of 136d (16.28 mg, 0.0600 mmol) in anhydrous DCM (1.0 mL) was added dropwise to a cold solution of thiocarbonyl diimidazole (21.39 mg, 0.1200 mmol) in anhydrous DCM (0.50 mL). The reaction was stirred at 0° C. for 1 h and then warmed to rt with stirring for 2 h. The mixture was concentrated down and the residue was flushed through a plug of silica gel with 10% EtOAc in hexanes. Concentration of the eluent afforded 136e.

Aufarbeitung

  1. temperaturewarmed to rt
  2. stirringwith stirring for 2 h
  3. concentrationThe mixture was concentrated down
  4. customthe residue was flushed through a plug of silica gel with 10% EtOAc in hexanes

Quellen und Nachweise

ORD-Eintrag
ord-3629865681d249a9b775d7348a6d1555
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08053450B2

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