Reaktion #55453

ord-9a555335c3d247efa8cafe6e3ea787c1

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solution is partially evaporated in vacuo
  2. 2
    Sonstigeto remove the hydrogen bromide
  3. 3
    WaschenThen it is washed with saturated sodium carbonate solution and with water
  4. 4
    Trocknendried over anhydrous sodium sulfate
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated in vacuo

Vorschrift

2-Phthalimidomethyl-5-propionylthiophene (39.3 g., 0.13 mole) is dissolved in methylene chloride 300 ml.) and bromine (20.8 g., 0.13 mole) is added dropwise with stirring over 3/4 hours at room temperature. The solution is partially evaporated in vacuo to remove the hydrogen bromide. Then it is washed with saturated sodium carbonate solution and with water, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. This affords 5-(2-bromopropionyl)-2-(phthalimidomethyl) thiophene as a pale beige solid (46.7 g.), m.p. 127°-130° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04220654uspto-grants-1980_09