Reaktion #51412
ord-7aeb8ae534b34973b7a463f3df84db89
Reaktionsgleichung
CH2Cl2
1-iodo-2-methylpropane
5-(N-Boc-amino)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one
Cs2CO3
→
5-amino-7-(2-methylpropyl)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one Hydrochloride
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter cooling to 23° C. the mixture
- 2Waschenwashed with several portions of brine
- 3Trocknendried over Na2SO4
- 4SonstigeThe 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).