Hydrochloride methanol → 2-Methyl-1-(piperazin-1-yl)propan-1-one

HRID 907792

Reaktionsgleichung

Reaktionsgleichung von HRID 907792
[C:1]([N:6]1[CH2:11][CH2:10][N:9](C(OC(C)(C)C)=O)[CH2:8][CH2:7]1)(=[O:5])[CH:2]([CH3:4])[CH3:3].Cl.CO>CO>[CH3:3][CH:2]([CH3:4])[C:1]([N:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1)=[O:5]

Komponenten

4

Edukt 2

HCID 21893726Hydrochloride methanolHCID 60708297tert-Butyl 4-isobutyrylpiperazine-1-carboxylate

Produkt 1

HCID 27614092-Methyl-1-(piperazin-1-yl)propan-1-oneAusbeute 132,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a stirred mixture of tert-butyl 4-isobutyrylpiperazine-1-carboxylate (6.8 g, 26.5 mmol) in methanol (15 mL) was added hydrochloride/methanol (30 mL, 3M)) at 0° C. After the addition, the mixture was allowed to stir at room temperature overnight. The mixture was concentrated to give 2-methyl-1-(piperazin-1-yl)propan-1-one (5.5 g, yield: 100%) as an off-white solid. 1H-NMR (400 MHz, CDCl3) δ: 3.82 (brs, 1H), 5.19 (s, 3H), 6.91-6.95 (m, 1H), 7.32-7.36 (m, 2H); LC-MS (ESI) m/z: 157(M+1)+.

Aufarbeitung

  1. additionAfter the addition
  2. concentrationThe mixture was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-f29e5b9fdc32420680bec4cd087ea250
Quelldatensatz
uspto-grants-2011_09
Patentnummer
US08012976B2

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