反応 #44464

反応方程式

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

収率 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

収率 80.0%

溶媒

DMF

反応条件

後処理

1. 1
   その他The resulting reaction mixture
2. 2
   抽出extracted with ethyl acetate (3×)
3. 3
   洗浄The organic layers were washed
4. 4
   乾燥After drying (MgSO4)
5. 5
   その他the solvents were removed under reduced pressure
6. 6
   その他The crude product was purified on silica with heptane/ethyl acetate 8:2

実験手順

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.

出典