反应详情

To the mixture of 5-Oxo-1-(toluene-4-sulfonyl)-2,3,4,5-tetrahydro-1H-benzo[b]azepine-4-carboxylic acid ethyl ester thus obtained, were added AcOH (2.4 l), conc.HCl (800 ml) and H2O (240 ml). The mixture was heated at reflux for 5 h and poured into ice water. The pH was adjusted to about 7-8 by adding diluted aqueous NaOH. The mixture was extracted with CH2Cl2. The organic layer was separated, dried over MgSO4, concentrated, and the residue was crystallized from the mixture (4:1 n-hexane:AcOEt) to give 1-(Toluene-4-sulfonyl)-1,2,3,4-tetrahydro-benzo[b]azepin-5-one (278 g, 60%) as a white powder.

1. customthus obtained
2. temperatureThe mixture was heated
3. temperatureat reflux for 5 h
4. extractionThe mixture was extracted with CH2Cl2
5. customThe organic layer was separated
6. dry with materialdried over MgSO4
7. concentrationconcentrated
8. customthe residue was crystallized from the mixture (4:1 n-hexane:AcOEt)