反应详情

温度

55 °C

A 2 L jacketed reactor is charged ammonium acetate (668 g, 8.67 mol) and the reactor is flushed with argon. Then 4-methyl-3-oxopentanoate (500 g, 3.47 mols) is charged followed by methanol (1.0 L). The mixture is agitated at 55° C. for 5 h and concentrated in vacuo to about 1 L and then cooled to about 20° C. A solution of iPrAc (1.5 L) is added and the organic phase is washed with water (2×1.0 L). The organic phase is concentrated to provide methyl 3-amino-4-methylpent-2-enoate (Int-2) as yellow oil (560 g, 68 wt %) in 76% yield, which is used directly in next step.

1. customthe reactor is flushed with argon
2. concentrationconcentrated in vacuo to about 1 L
3. temperaturecooled to about 20° C
4. additionA solution of iPrAc (1.5 L) is added
5. washthe organic phase is washed with water (2×1.0 L)
6. concentrationThe organic phase is concentrated