反应详情

温度

100 °C

A mixture of 4-(pyridin-2-yloxymethyl)-benzaldehyde described in Preparation Example 1-4-2 (26.8 g, 126 mmol), nitro methane (34 mL, 630 mmol), ammonium acetate (19 g, 252 mmol) and acetic acid (90 mL) was stirred at 100° C for 90 minutes. To the reaction solution were added ethyl acetate and water to carry out liquid separation. The organic layer thereof was separated, washed with water (five times) and saturated sodium bicarbonate water (once), dried over anhydrous magnesium sulfate and then filtered. The filtrate thereof was concentrated under a reduced pressure to obtain the title compound (31 g) as a crude product.

1. customliquid separation
2. customThe organic layer thereof was separated
3. washwashed with water (five times) and saturated sodium bicarbonate water (once),
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. concentrationThe filtrate thereof was concentrated under a reduced pressure