反应详情

温度

60 °C

Ethylene chlorohydrin (16.10 g, 0.2M) was added to a solution of 2-hydroxy-3-benzyl-5,6,7,8-tetrahydroquinoxaline (9.60 g, 40 mM) in dilute aqueous 5N NaOH (40 ml) and t-butanol (120 ml), and stirred at 60° C. for 3 hours. The t-butanol was distilled off in vacuo. The residue was extracted three times with chloroform, dried with anhydrous sodium sulfate and concentrated in vacuo. The residue was charged on a column of silica-gel (C-200, 220 g) packed with chloroform, and eluted with chloroform-methanol (200:1) to obtain compound 643 (10.90 g, yield: 83.8%).

1. distillationThe t-butanol was distilled off in vacuo
2. extractionThe residue was extracted three times with chloroform
3. dry with materialdried with anhydrous sodium sulfate
4. concentrationconcentrated in vacuo
5. additionThe residue was charged on a column of silica-gel (C-200, 220 g)
6. washeluted with chloroform-methanol (200:1)