Reaktion #42889

ord-b604834c7358483795593421fbc68b98

Reaktionsbedingungen

Temperatur
-15°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto warm up to room temperature
  2. 2
    Waschenthe solution was washed twice with water
  3. 3
    Trocknendried over sodium sulfate
  4. 4
    Einengenconcentrated in vacuo
  5. 5
    SonstigeThe residue was purified by column chromatography

Vorschrift

To a suspension of 4-amino-thiophene-3-carboxylic acid methyl ester (2.0g) in dichloromethane (25 mL) was added 2-chloropropionyl chloride (1.13 mL). The reaction mixture was then cooled down to −15° C. and a solution of triethylamine (3.2 mL) in dichloromethane (5 mL) was slowly added over 30 minutes. After such time the reaction mixture was allowed to warm up to room temperature, and the solution was washed twice with water, dried over sodium sulfate and then concentrated in vacuo. The residue was purified by column chromatography to yield the title compound as a light yellow solid (2.1g, 82%). MS (EI): 247.0.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732452B2uspto-grants-2010_06