反应详情

To 50 ml of DMF was added 5.0 g (0.0126 mol) of product of Example 28, followed by 1.27 g (0.0126 mol) of triethylamine and 1.74 g (0.0126 mol) of K2CO3. To this mixture was added 0.922 g (0.0161 mol) of propyleneimine. This reaction mixture was stirred under N2 for 48 hours at room temperature. The reaction mixture was then poured into H2O and extracted with diethyl ether. The ether phase was then washed with H2O, and dried over MgSO4. The dry ether phase was then concentrated in vacuo to a crude yield of 4.8 g of a brown oil. This oil was kugelrohr distilled at 105° C./53 Pa, to yield 4.0 g of a yellow oil (76%) nD25 1 4763.

1. extractionextracted with diethyl ether
2. washThe ether phase was then washed with H2O
3. dry with materialdried over MgSO4
4. concentrationThe dry ether phase was then concentrated in vacuo to a crude yield of 4.8 g of a brown oil
5. distillationThis oil was kugelrohr distilled at 105° C./53 Pa