Acetic acid, ion(1-) (8CI,9CI) → N-3-methoxypropyl-N-ethylguanidine

HRID 763

反应方程式

HRID 763 反应方程式
[CH2:1]([NH:3][CH2:4][CH2:5][CH2:6][O:7][CH3:8])[CH3:2].C(O)(=O)C.[N:13]#[C:14][NH2:15].C([O-])(=O)C>>[CH3:8][O:7][CH2:6][CH2:5][CH2:4][N:3]([CH2:1][CH3:2])[C:14]([NH2:15])=[NH:13]

参与物

5

反应物 4

HCID 175Acetic acid, ion(1-) (8CI,9CI)HCID 176醋酸HCID 9864氰胺HCID 12238051N-ethyl-3-methoxypropan-1-amine

产物 1

HCID 21259568N-3-methoxypropyl-N-ethylguanidine收率 50%

反应条件

温度
90 °C

实验过程

3.00 g (25.6 mmol) of N-ethyl-3-methoxypropylamine and 1.54 g (25.6 mmol) of acetic acid were placed in a 50 ml two neck flask. While heating the flask in a 90° C. oil bath, 1.08 g (25.6 mmol) of cyanamide was added. After 12 hours of the reaction, the product was purified by a silica gel column chromatography (eluent, chloroform/ethanol=1/2 containing 0.5% acetic acid) to obtain 2.80 g of the title compound (wax-like, 12.8 mmol, 50.0% in yield) in the form of acetate. Results of the analysis of this compound are as follows.

后处理

  1. customAfter 12 hours of the reaction
  2. customthe product was purified by a silica gel column chromatography (eluent, chloroform/ethanol=1/2 containing 0.5% acetic acid)

来源与证据

ORD记录
ord-0b3cb71fbde54da5a7c439131d7d2319
来源数据集
uspto-grants-1998_03
专利号
US05723133

关联笔记

加载中…