반응 #44464

반응 방정식

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

수율 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

수율 80.0%

용매

DMF

반응 조건

후처리

1. 1
   기타The resulting reaction mixture
2. 2
   추출extracted with ethyl acetate (3×)
3. 3
   세척The organic layers were washed
4. 4
   건조After drying (MgSO4)
5. 5
   기타the solvents were removed under reduced pressure
6. 6
   기타The crude product was purified on silica with heptane/ethyl acetate 8:2

실험 절차

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.

출처