反应详情

温度

120 °C

(S)-3-(hydroxymethyl)-6a,7,8,9-tetrahydropyrido[3,2-e]pyrrolo[1,2-a]pyrazin-6(5H)-one (300 mg, 1.368 mmol), N-cyclopropyl-4-(piperazin-1-yl)benzamide (336 mg, 1.368 mmol), (cyanomethyl)trimethylphosphonium iodide (499 mg, 2.053 mmol) and N,N-diisopropylethylamine (1195 μl, 6.84 mmol) were suspended in propionitrile (Volume: 4109 μl) and heated in a closed vial at 120° C. for 2 h. The reaction mixture became a dark brown solution. It was cooled to room temperature, concentrated in vacuo, dissolved in DMSO (2 mL) and purified using HPLC (NH4HCO3 buffered, 20-70% ACN in water). The fractions were concentrated in vacuo and the resulting solid was recrystallized from water—MeOH (1:1, 15 mL), and then from MeOH:EtOH:water (1:1:1, 10 mL), washed with water (3 mL) and dried in vacuum to give a light green solid.

1. temperatureIt was cooled to room temperature
2. concentrationconcentrated in vacuo
3. dissolutiondissolved in DMSO (2 mL)
4. custompurified
5. concentrationThe fractions were concentrated in vacuo
6. customthe resulting solid was recrystallized from water—MeOH (1:1, 15 mL)
7. washfrom MeOH:EtOH:water (1:1:1, 10 mL), washed with water (3 mL)
8. customdried in vacuum
9. customto give a light green solid