Reaktion #71418

ord-b6f1359851554a6e8633af1cffc9717a

Reaktionsgleichung

CCOC(=O)C(C)(C)Br
ethyl-2-bromoisobutyrate
NCCN
ethylene diamine
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CC1(C)NCCNC1=O
title compound
Ausbeute 68.8%
CC1(C)NCCNC1=O
3,3-Dimethyl-piperazin-2-one
Ausbeute 68.8%

Lösungsmittel

Reaktionsbedingungen

Temperatur
115°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled
  2. 2
    Filtrationfiltered
  3. 3
    EinengenThe filtrate was concentrated
  4. 4
    Sonstigethe residue triturated in Et2O

Vorschrift

A solution of ethyl-2-bromoisobutyrate (24 mL, 161 mmol) in toluene (150 mL) was added to a mixture of ethylene diamine (70 mL, 1046 mmol, 6.5 equiv) and potassium carbonate (24.4 g, 177 mmol, 1.1 equiv) in toluene (150 mL). The reaction mixture was heated for 20 h at 115° C., cooled and filtered. The filtrate was concentrated and the residue triturated in Et2O to afford 14.2 g of the title compound as a yellow solid: ESI-MS: 129.1 [M+H]+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08536175B2uspto-grants-2013_09