Réaction #51413

ord-aa5db1a52ef141b09e1c109095bb69a8

Solvants

Conditions de réaction

Température
60°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    TempératureAfter cooling to 23° C. the mixture
  2. 2
    Lavagewashed with several portions of brine
  3. 3
    Séchagedried over Na2SO4
  4. 4
    AutreThe title compound was purified by chromatography (SiO2, CHCl3)

Mode opératoire

A solution of 5-(N-Boc-amino)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one (1.03, 3.08 mmol) (Example 7-E) in DMF was treated with Cs2CO3 (1.10 g, 3.39 mmol) and warmed to 60° C. To the reaction mixture was added bromomethyl acetate (0.321 ml, 3.39 mmol) (Aldrich) and stirring continued for 17 h. After cooling to 23° C. the mixture was diluted with CH2Cl2, washed with several portions of brine and dried over Na2SO4. The title compound was purified by chromatography (SiO2, CHCl3).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US06849650B2uspto-grants-2005_02