反应详情

1-(4-Nitrophenoxy)-2,3-epoxypropane (Reference Example 1-B, 4.3 g) was dissolved in methanol (30 ml) and DMF (10 ml). Dimethylamine (2M solution in methanol, 17 ml) was added and the mixture was stirred at ambient temperature overnight. The reaction mixture was evaporated to dryness and the residue was dissolved in saturated sodium bicarbonate solution and ethyl acetate. The ethyl acetate layer was separated and washed twice with saturated brine, dried over anhydrous sodium sulphate, filtered and evaporated to yield an oil that slowly crystallised under high vacuum (4.79 g, 89.9%). NMR: (CDCl3, 300 MHz) 2.33 (s, 6H), 2.98 (m, 1H), 2.54 (m, 1H), 4.00 (m,3 H), 7.00 (d, 2H), 8.20 (d, 2H); M.S.: (ES+) 241 (MH+).

1. customThe reaction mixture was evaporated to dryness
2. dissolutionthe residue was dissolved in saturated sodium bicarbonate solution
3. customThe ethyl acetate layer was separated
4. washwashed twice with saturated brine
5. dry with materialdried over anhydrous sodium sulphate
6. filtrationfiltered
7. customevaporated
8. customto yield an oil that
9. customslowly crystallised under high vacuum (4.79 g, 89.9%)