반응 #1174

반응 방정식

K2CO3

1-Benzyloxycarbonyl-4-phthalimidylpiperidine

hydrazine monohydrate

→

4-amino-1-benzyloxycarbonylpiperidine

수율 85.0%

용매

ethanol

Brine

반응 조건

후처리

1. 1
   추출the mixture was extracted with 5% MeOH/CHCl3 (3×)
2. 2
   세척The combined extracts were washed with 2N aq. HCl, 2N aq. NaOH, brine solution
3. 3
   건조dried over Na2SO4
4. 4
   농축concentrated

실험 절차

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.

출처