反应 #1174

ord-2cac9a20d7c04458add12877e56c0bdb

反应方程式

O=C([O-])[O-].[K+].[K+]
K2CO3
O=C(OCc1ccccc1)N1CCC(N2C(=O)c3ccccc3C2=O)CC1
1-Benzyloxycarbonyl-4-phthalimidylpiperidine
NN.O
hydrazine monohydrate
NC1CCN(C(=O)OCc2ccccc2)CC1
4-amino-1-benzyloxycarbonylpiperidine
收率 85.0%

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723490uspto-grants-1998_03