Reaktion #11709

ord-b437499df33d48f784286683f8fd74db

Lösungsmittel

Reaktionsbedingungen

Temperatur
95°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool to ambient temperature
  2. 2
    Extraktionextracted with diethyl ether
  3. 3
    TrocknenThe organic layer was dried over magnesium sulfate
  4. 4
    Filtrationfiltered
  5. 5
    Einengenconcentrated in vacuo

Vorschrift

To a solution of sodium hydroxide (6.6 g, 160 mmol) in water (45 mL) was added 4-chloro-2-methoxy-phenol (2.0 mL, 16 mmol) and chloroacetic acid (7.7 g, 81 mmol). The resulting mixture was heated to 95° C. and stirred for three hours. The reaction was allowed to cool to ambient temperature and slowly acidified with concentrated hydrochloric acid (10 mL) until the mixture became a solution and then extracted with diethyl ether. The organic layer was dried over magnesium sulfate, filtered and concentrated in vacuo to give the title compound (4.16 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07098212B2uspto-grants-2006_08