Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Edukt | Phenylmethyl 4-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)-1-piperidinecarboxylate | HCID 21831105 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Sodium chloride; water | HCID 57417360 | — |
| Produkt | 4-Amino-1-N-Cbz-piperidine | HCID 17846640 | 85% |
Reaktionsschritte
1-Benzyloxycarbonyl-4-phthalimidylpiperidine (1.50 g, 4.27 mmol), prepared in Example 16B, was taken up in 20 mL of ethanol. To this solution was added hydrazine monohydrate (35 mL, 700 mmol) and this mixture was heated at 100° C. for 3 h. Brine solution (40 mL) and 10% aq. K2CO3 (60 mL) were added and the mixture was extracted with 5% MeOH/CHCl3 (3×). The combined extracts were washed with 2N aq. HCl, 2N aq. NaOH, brine solution, dried over Na2SO4 and concentrated to give 0.847 g, (85%) of 4-amino-1-benzyloxycarbonylpiperidine. [1H]-NMR(CDCl3) consistent with structure.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US05723490 |
|---|
| Quelldatensatz | uspto-grants-1998_03 |
|---|
| ORD ID | ord-2cac9a20d7c04458add12877e56c0bdb |
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| Quellennotiz | uspto-grants-1998_03 |
|---|
