Methanol → Methyl 4-aminopiperidine-4-carboxylate dihydrochloride

Into a heterogeneous mixture of 4-amino-4-carboxypiperidine dihydrochloride (61.0 g, 0.34 mmol) in methanol (600 mL) is bubbled hydrogen chloride gas at room temperature. The reaction mixture is concentrated to dryness in vacuo, dissolved in 1,4-dioxane (200 mL), and concentrated in vacuo. The residue is redissolved in methanol (1600 mL) into which hydrogen chloride gas is bubbled for 45 minutes. The reaction mixture is refluxed for 18 hours. Most of the solvent is then evaporated, the product is collected by filtration, and washed with ethyl acetate to give 4-amino-4-carbomethoxypiperidine dihydrochloride.

1. customis bubbled hydrogen chloride gas at room temperature
2. concentrationThe reaction mixture is concentrated to dryness in vacuo
3. dissolutiondissolved in 1,4-dioxane (200 mL)
4. concentrationconcentrated in vacuo
5. dissolutionThe residue is redissolved in methanol (1600 mL) into which hydrogen chloride gas
6. customis bubbled for 45 minutes
7. temperatureThe reaction mixture is refluxed for 18 hours
8. customMost of the solvent is then evaporated
9. filtrationthe product is collected by filtration
10. washwashed with ethyl acetate

ORDレコード

ord-73b43d5876ec4f5d987e391af8b35bca

出典データセット

uspto-grants-1996_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05552419