Réaction #44464

Équation de réaction

water

ethyl bromoacetate

triethylamine

trans-7-chloro-1,2,3,4,10,14b-hexahydro-10-methyldibenzo[b,f]pyrido[1,2-d][1,4]-diazepin-1-ylamine

→

title compound

Rendement 80.0%

Ethyl trans-[(7-chloro-1,2,3,4,10,14b-hexahydro-10-methyldibenzo[b,f]pyrido[1,2-d][1,4]diazepin-1-yl)amino]acetate

Rendement 80.0%

Solvants

DMF

Conditions de réaction

Traitement

1. 1
   AutreThe resulting reaction mixture
2. 2
   Extractionextracted with ethyl acetate (3×)
3. 3
   LavageThe organic layers were washed
4. 4
   SéchageAfter drying (MgSO4)
5. 5
   Autrethe solvents were removed under reduced pressure
6. 6
   AutreThe crude product was purified on silica with heptane/ethyl acetate 8:2

Mode opératoire

To a suspension of trans-7-chloro-1,2,3,4,10,14b-hexahydro-10-methyldibenzo[b,f]pyrido[1,2-d][1,4]-diazepin-1-ylamine (100 mg, 0.25 mmol) in DMF (2 mL) was added ethyl bromoacetate (56 μl, 0.51 mmol) and triethylamine (107 ul, 0.76 mmol). The resulting reaction mixture was heated to 60° C. and stirred for 5 h. The mixture was poured into water and extracted with ethyl acetate (3×). The organic layers were washed with sat (aq) NaHCO3 and brine. After drying (MgSO4), the solvents were removed under reduced pressure. The crude product was purified on silica with heptane/ethyl acetate 8:2 to afford 80 mg (80%) of the title compound.

Source