1-Methylpiperazine → 4-Methylpiperazine-1-carboxamide

HRID 2100424Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2100424
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.C[Si]([N:12]=[C:13]=[O:14])(C)C>C(O)(C)C>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:13]([NH2:12])=[O:14])[CH2:4][CH2:3]1

Komponenten

4

Edukt 2

HCID 531671-MethylpiperazineHCID 70696Trimethylsilyl isocyanate

Produkt 1

HCID 4102614-Methylpiperazine-1-carboxamideAusbeute 121,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

To a stirred solution of 1-methylpiperazine (1.66 mL, 15 mmol) in isopropanol (30 mL) at rt was added trimethylsilylisocyanate (2.8 mL, 21 mmol) and the resulting solution stirred overnight. The volatiles were removed in vacuo to give 4-methyl-piperazine-1-carboxylic acid amide (2.6 g, quant.) as an oil which slowly crystallised on standing; 1H-NMR (300 MHz, CDCl3) 4.62 (2H, s), 3.40 (4H, t), 2.39 (4H, t), 2.29 (3H, s); m/z (ES+) 143 [M+H]+.

Aufarbeitung

  1. customThe volatiles were removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-0562800d7a3e44cfb10aa41234c33b19
Quelldatensatz
uspto-grants-2009_08
Patentnummer
US07572794B2

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