反应详情

A solution of 0.5 g (1.9 mmol) of 8-chloro-5,10-dihydro-dibenzo[b,e][1,4]diazepin-11-thione in 10 mL of 2-ethoxyethanol was treated with 0.46 g (3.8 mmol) of 3-(2-aminoethyl)pyridine and heated at reflux overnight. The solvent was removed under reduced pressure and the residue taken up in EtOAc and washed five times with H2O, then saturated NaCl solution. Drying over MgSO4 and removal of the solvent under reduced pressure gave the crude product. Recrystallization from acetone/water gave 0.49 g (74% yield) of the product as a yellow solid, mp 195-196° C. The structure was confirmed by NMR and mass spectroscopy. (m+H)+ =349.

1. temperatureheated
2. temperatureat reflux overnight
3. customThe solvent was removed under reduced pressure
4. washwashed five times with H2O
5. dry with materialDrying over MgSO4 and removal of the solvent under reduced pressure
6. customgave the crude product
7. customRecrystallization from acetone/water