Dimethylformamide → HCID 178420383, Verbindung

HRID 1798820

Reaktionsgleichung

Reaktionsgleichung von HRID 1798820
C[Si]([N:5]=[N+:6]=[N-:7])(C)C.CN(C=O)C.[CH2:13]([O:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]#[CH:28])=[CH:23][CH:22]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>[Cu]I.CO>[CH2:13]([O:20][C:21]1[CH:22]=[CH:23][C:24]([C:27]2[N:5]=[N:6][NH:7][CH:28]=2)=[CH:25][CH:26]=1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

Komponenten

6

Edukt 3

HCID 6228DimethylformamideHCID 78378AzidotrimethylsilaneHCID 14903234'-Benzyloxyphenyl acetylene

Produkt 1

HCID 178420383HCID 178420383, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)KatalysatorHCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

Trimethylsilyl azide (415 mg, 3.6 mmol) was added to a DMF (4.3 mL) and MeOH (0.48 mL) solution containing CuI (22.9 mg, 0.12 mmol) and 1-(benzyloxy)-4-ethynylbenzene (500 mg, 2.4 mmol) under Ar in a pressure tube (caution: build-up of pressure possible; use a safety shield). The reaction mixture was stirred at 100° C. for 12 h. The mixture was cooled to room temperature and filtered through a short silica gel pad and concentrated. The residue was purified by recrystallization from DCM.

Aufarbeitung

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationfiltered through a short silica gel pad
  3. concentrationconcentrated
  4. customThe residue was purified by recrystallization from DCM

Quellen und Nachweise

ORD-Eintrag
ord-57629a30725e489cb4bcd5f5837562dd
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08343990B2

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