Reaktion #1670091

ord-ec5ce75b1f9b495f942b0995ee848ffd

Lösungsmittel

Reaktionsbedingungen

Temperatur
-20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was then warmed to room temperature
  2. 2
    FiltrationThe residue was filtered off with suction
  3. 3
    Extraktionextracted with THF
  4. 4
    Einengenthe filtrates were concentrated

Vorschrift

2-(N-Boc-Aminomethyl)-5-methylthiazole-4-carboxylic acid (6.8 g, 25 mmol) was dissolved in THF (100 ml), and triethylamine (2.53 g, 25 mmol) was added. After the mixture had been cooled to −20° C., a solution of isobutyl chloroformate (3.41 g, 25 mmol) in THF (10 ml) was added dropwise. After the mixture had been stirred for 30 minutes at −20° C., ammonia gas was passed into the pale brown suspension for 45 minutes. The mixture was then warmed to room temperature. The residue was filtered off with suction and extracted with THF, and the filtrates were concentrated.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06740647B1uspto-grants-2004_05