Reaktion #1174

Reaktionsgleichung

K2CO3

1-Benzyloxycarbonyl-4-phthalimidylpiperidine

hydrazine monohydrate

→

4-amino-1-benzyloxycarbonylpiperidine

Ausbeute 85.0%

Lösungsmittel

ethanol

Brine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe mixture was extracted with 5% MeOH/CHCl3 (3×)
2. 2
   WaschenThe combined extracts were washed with 2N aq. HCl, 2N aq. NaOH, brine solution
3. 3
   Trocknendried over Na2SO4
4. 4
   Einengenconcentrated

Vorschrift

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.

Quelle