Reaktion #51412

ord-7aeb8ae534b34973b7a463f3df84db89

Reaktionsgleichung

ClCCl
CH2Cl2
CC(C)CI
1-iodo-2-methylpropane
CC(C)(C)OC(=O)NN1C(=O)Cc2ccccc2-c2ccccc21
5-(N-Boc-amino)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one
O=C([O-])[O-].[Cs+].[Cs+]
Cs2CO3
CC(C)CC1C(=O)N(N)c2ccccc2-c2ccccc21.Cl
5-amino-7-(2-methylpropyl)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one Hydrochloride

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling to 23° C. the mixture
  2. 2
    Waschenwashed with several portions of brine
  3. 3
    Trocknendried over Na2SO4
  4. 4
    SonstigeThe title compound was purified by chromatography (SiO2, CHCl3/MeOH 9:1)

Vorschrift

A solution of 5-(N-Boc-amino)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one (0.2 g, 0.617 mmol) (Example 7-E) in DMF was treated with Cs2CO3 (0.22 g, 0.678 mmol) and warmed to 60° C. To the reaction mixture was added 1-iodo-2-methylpropane (0.078 ml, 0.678 mmol) 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/MeOH 9:1).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06849650B2uspto-grants-2005_02