反応 #1174

反応方程式

K2CO3

1-Benzyloxycarbonyl-4-phthalimidylpiperidine

hydrazine monohydrate

→

4-amino-1-benzyloxycarbonylpiperidine

収率 85.0%

溶媒

ethanol

Brine

反応条件

後処理

1. 1
   抽出the mixture was extracted with 5% MeOH/CHCl3 (3×)
2. 2
   洗浄The combined extracts were washed with 2N aq. HCl, 2N aq. NaOH, brine solution
3. 3
   乾燥dried over Na2SO4
4. 4
   濃縮concentrated

実験手順

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.

出典