تفاعل #44464

معادلة التفاعل

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

المردود 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

المردود 80.0%

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   أخرىThe resulting reaction mixture
2. 2
   استخلاصextracted with ethyl acetate (3×)
3. 3
   غسيلThe organic layers were washed
4. 4
   تجفيفAfter drying (MgSO4)
5. 5
   أخرىthe solvents were removed under reduced pressure
6. 6
   أخرىThe crude product was purified on silica with heptane/ethyl acetate 8:2

الإجراء التجريبي

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.

المصدر