Reaktion #303090

ord-205044f7b146465e85e1646f1f02c17f

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGThe reaction mixture was stirred for 2 hours
  2. 2
    Waschenwashed sequentially with water, 1 N hydrochloric acid and saturated sodium bicarbonate
  3. 3
    Trocknendried with magnesium sulfate
  4. 4
    Filtrationfiltered
  5. 5
    Einengenconcentrated

Vorschrift

Triethylamine (1.63 g) was added to a suspension of β-alanine methyl ester hydrochloride (2.25 g) in dichloromethane (10 mL) and the reaction mixture was stirred for 30 minutes. After addition of pyridine (1.27 g) the reaction mixture was cooled to 0° C. A solution of 2-chloropropionyl chloride (2.04 g) in dichloromethane (10 mL) was added dropwise for 20 minutes. The reaction mixture was stirred for 2 hours, washed sequentially with water, 1 N hydrochloric acid and saturated sodium bicarbonate, dried with magnesium sulfate, filtered, and concentrated to give yellow oil (2.9 g, yield 93%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08193198B2uspto-grants-2012_06