反应详情

温度

80 °C

A mixture of potassium (bromomethyl)trifluoroborate (1.20 g, 5.38 mmol) and (R)-4-N-Boc-2-methyl-piperazine (1.166 g, 5.65 mmol) in THF (7.00 mL) was heated at 80° C. under nitrogen for 24 h. After cooling, the mixture was concentrated, re-dissolved in acetone (125 mL) and treated with K2CO3 (1 eq). The suspension was stirred for 30 min and filtered through a short plug of Celite® (diatomaceous earth), washing with additional acetone and the combined organic phases were concentrated to give potassium (R)-((4-(tert-butoxycarbonyl)-2-methylpiperazin-1-yl)methyl)trifluoroborate as a pale yellow foam (1.627 g, 94%). 19F-NMR (377 MHz, d6-acetone) δ −141.36.

1. temperatureAfter cooling
2. concentrationthe mixture was concentrated
3. dissolutionre-dissolved in acetone (125 mL)
4. filtrationfiltered through a short plug of Celite® (diatomaceous earth)
5. washwashing with additional acetone
6. concentrationthe combined organic phases were concentrated