反応 #156814

反応方程式

(S)-3-(hydroxymethyl)-7,8,9,10-tetrahydro-5H-dipyrido[1,2-a:3′,2′-e]pyrazin-6(6aH)-one

(cyanomethyl)trimethylphosphonium iodide

DIEA

N-ethyl-4-(piperazin-1-yl)benzamide

→

(S)—N-ethyl-4-(4-((6-oxo-6,6a,7,8,9,10-hexahydro-5H-dipyrido[1,2-a:3′,2′-e]pyrazin-3-yl)methyl)piperazin-1-yl)benzamide

反応条件

後処理

1. 1
   その他The crude reaction
2. 2
   温度was cooled to RT
3. 3
   ろ過filtered
4. 4
   その他The resulting solid were collected
5. 5
   温度heated
6. 6
   温度to reflux
7. 7
   温度cooled to RT
8. 8
   ろ過filtered
9. 9
   洗浄The resulting material was rinsed with EtOH
10. 10
    その他to give a white solid

実験手順

To a suspension of (S)-3-(hydroxymethyl)-7,8,9,10-tetrahydro-5H-dipyrido[1,2-a:3′,2′-e]pyrazin-6(6aH)-one (800 mg, 3.43 mmol) was added (cyanomethyl)trimethylphosphonium iodide (1000 mg, 4.12 mmol) and DIEA (1797 μl, 10.29 mmol) and N-ethyl-4-(piperazin-1-yl)benzamide (800 mg, 3.43 mmol)). The vial was heated to 90° C. for 16 hours. The crude reaction was cooled to RT and filtered. The resulting solid were collected and suspended in EtOH (24 mL), heated to reflux, then cooled to RT and filtered. The resulting material was rinsed with EtOH to give a white solid.

出典