反应详情

温度

130 °C

Piperidinemethanol (10.7 g, 93 mmol) is dissolved in DMA (60 mL), treated with 2-chloro-5-ethylpyrimidine (14.57 g, 102 mmol) and K2CO3 (19.3 g, 140 mmol) and heated to 130° C. overnight. The solid is filtered, washed with DMA and discarded. The filtrate is evaporated and the crude purified by flash chromatography (EtOAc/hexanes gradient) to afford (1-(5-ethylpyrimidin-2-yl)piperidin-4-yl)methanol A1a as yellow oil: 1H-NMR (400 MHz, CDCl3) δ=8.16 (s, 2H), 4.75-4.72 (m, 2H), 3.53 (d, J=6.0 Hz, 2H), 2.91-2.83 (m, 2H), 2.45 (q, J=7.6 Hz, 2H), 1.84-1.73 (m, 3H), 1.27-1.20 (m, 2H), 1.18 (t, J=7.6 Hz, 3H); MS calcd. for [M+H]+ C12H20N3O: 222.1. found: 222.1.

1. filtrationThe solid is filtered
2. washwashed with DMA
3. customThe filtrate is evaporated
4. customthe crude purified by flash chromatography (EtOAc/hexanes gradient)