HRID1060208
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To isophoronediamine (139.23 g, 0.819 mol) in methanol (700 ml) was slowly added with stirring ethyl butyroacetate (262.32 g, 1.660 mol) in methanol (700 ml) over 45 minutes, during which the temperature decreased slightly from 24° C. to 23° C. The reaction mixture was allowed to stand at 22° C. overnight (16 h). Further methanol was added, and removal of solvent and drying (91° C./100 Pa) gave 1-(1-ethoxycarbonyl-2-pent-1-enylamino)-3-(1-ethoxycarbonyl-2-pent-1-enylaminomethyl)-3,5,5-trimethylcyclohexane (EEMTCH formula shown below) as a clear light yellow pourable syrup (356.74 g, 97%), identified by 1H-NMR, 13C-NMR, FT-IR and Raman spectra.
WORKUP
后处理
- customdecreased slightly from 24° C. to 23° C
- custom(16 h)
- customremoval of solvent
- customdrying (91° C./100 Pa)