Reaktion #413588

ord-12dc5448f6c04d40be0466b38261f8b2

Reaktionsgleichung

Nc1nc(C[C@H](N)C(=O)O)cs1
3-(2-Amino-4-thiazolyl)alanine
N[C@@H](CCC(=O)O)C(=O)O
L-glutamic acid
CO
Methanol
N[C@@H](CCC(=O)O)C(=O)O.Nc1nc(C[C@H](N)C(=O)O)cs1
3-(2-amino-4-thiazolyl)-L-alanine L-glutamic acid salt

Lösungsmittel

Reaktionsbedingungen

Temperatur
25°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto crystallize the salt
  2. 2
    Filtrationthe product is filtered
  3. 3
    Waschenwashed with 40 L of methanol
  4. 4
    SonstigeThe product is dried at 40° C. under vacuum

Vorschrift

DL-3-(2-Amino-4-thiazolyl)alanine, 41.8 kg (223 mol) (Silberg, A., et al, Chemische Berichte, Vol. 97, pages 1767-69 (1964)) and 26.3 kg (179 mol) of L-glutamic acid are dissolved in 620 L of water at 60° C. Methanol (620 L) is added to the solution and the solution is cooled to 25° C. to crystallize the salt. After stirring for 2 to 3 hours at 25° C., the product is filtered and washed with 40 L of methanol. The product is dried at 40° C. under vacuum to give 37.6 kg of 3-(2-amino-4-thiazolyl)-L-alanine L-glutamic acid salt as a white solid. Infrared spectrum (IR) (mineral oil): 2927 (s, br), 1643 (s), 1605 (s), 1548 (s), 1407 (sh) cm-1.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05268483uspto-grants-1993_12