Reaktion #610739

ord-786e68a5ac7e44a9b303b49a6c676aac

Lösungsmittel

Reaktionsbedingungen

Temperatur
200°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with ethyl acetate
  2. 2
    EinengenThe organic layer was concentrated
  3. 3
    Sonstigepurified by column chromatography on silica gel (100% hexane)

Vorschrift

DBU (1.21 g, 8.00 mmol) was added to a stirred solution of 6-bromo-benzo[b]thiophene-2-carboxylic acid (I-25b: 2.4 g, 8.85 mmol) in DMA (4 mL) at room temperature and the resulting mixture was heated in microwave at 200° C. for 1 hour. The reaction was monitored by TLC (50% ethyl acetate in hexane). The reaction mixture was acidified with 1N HCl and extracted with ethyl acetate. The organic layer was concentrated and purified by column chromatography on silica gel (100% hexane) to afford 320 mg of the product (78% yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09339501B2uspto-grants-2016_05