反应详情

温度

-78 °C

Add anhydrous DMSO (3.57 mL, 50.25 mmol) in anhydrous dichloromethane (68.0 mL). Cool to −78° C. and stir. Add oxalyl chloride (2M in dichloromethane, 12.06 mL, 24.125 mmol) dropwise. Stir at −78° C. for 30 minutes. Add (1,4-dibenzyl-piperazin-2-yl)-ethanol (6.241 g, 20.1 mmol) in dichloromethane (12.0 mL) and stir. After 1 hour, add triethylamine (14.01 mL, 100.5 mmol) and stir for another 1 hour. Allow the reaction mixture gradually warm to ambient temperature. Add saturated ammonium chloride. (200 mL). Exact aqueous portion with ethyl acetate three times. Combine the organic solution, dry over sodium sulfate, filter, and concentrate under reduced pressure to give crude residue. Purify the residue by flash chromatography, eluting with 2M ammonia in methanol:dichloromethane (5:95) to give the title compound: mass spectrum (m/e):309.03 (M+1).

1. stirringStir at −78° C. for 30 minutes
2. stirringstir for another 1 hour
3. temperaturegradually warm to ambient temperature
4. dry with materialCombine the organic solution, dry over sodium sulfate
5. filtrationfilter
6. concentrationconcentrate under reduced pressure
7. customto give crude residue
8. customPurify the residue by flash chromatography
9. washeluting with 2M ammonia in methanol:dichloromethane (5:95)