反应详情

温度

-40 °C

1-Azabicyclo[2.2.1]hept-4-yl-N-methoxy-N-methyl carboxamide (D21) (10 g, 0.054 mole) was dissolved in dry THF (250 ml) under nitrogen cooled to -40° C. and treated with methyl lithium in ether (55 ml, 1 molar, 0.055 moles). The solution was allowed to warm to room temperature over a period of 1 h. Acetic acid (3.3 ml, leq) was added and the solution concentrated in vacuo to a gum. The residue was partitioned between chloroform and saturated aqueous potassium carbonate solution. The organic phase was separated, dried over sodium sulphate and concentrated in vacuo to a gum which was distilled in vacuo to afford 4-acetyl-1-azabicyclo[2.2.1]heptane (D22) (5.15 g, 0.037 mole, 68%).

1. temperatureto warm to room temperature over a period of 1 h
2. concentrationthe solution concentrated in vacuo to a gum
3. customThe residue was partitioned between chloroform and saturated aqueous potassium carbonate solution
4. customThe organic phase was separated
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated in vacuo to a gum which
7. distillationwas distilled in vacuo