Reaktion #79143

ord-35e3eb27375e43f0be23b39b8d7563a3

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONA mixture of the compound
  2. 2
    Sonstigeprepared
  3. 3
    Temperaturwas cooled
  4. 4
    Sonstigeto about 20-25° C
  5. 5
    Sonstigethe in situ HPLC yield

Vorschrift

A mixture of the compound prepared as described in Preparation 1 (8.46 grams) and the acid chloride prepared as described in Preparation 3 (10.0 grams) in methylene chloride (350 mL) was cooled:to about 20-25° C. The cool mixture was treated with boron trichloride (2.6 mL), and the resulting mixture mechanically stirred. The reaction was monitored by HPLC using the assay described above. After 85 minutes, the in situ HPLC yield based on a 6-methoxy-2-(4-methoxyphenyl)-3-[4-(2-piperidinylethoxy)benzoyl]benzo[b]thiophene standard was 88%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06713494B1uspto-grants-2004_03