反应详情

温度

50 °C

To a slurry containing 5.0 g of (R)-4-carbobenzyloxypiperazine-2-carboxylic acid, 4.2 g of 1,2-dichloro-fluoro-5-nitrobenzene, 85 mL of water and 170 mL of dimethylformamide is added slowly 5.3 mL of triethylamine. The solution is heated to 50° C. for 5 hours, then at ambient temperature overnight. The dark orange solution is concentrated under reduced pressure (1-2 mm, <50° C.) to an orange oily residue. This oil is dissolved in 400 mL of ethyl acetate and washed with 100 mL of 1 N HCl (2×), with 150 mL of water (2×), and 100 mL of brine. The organic layer is dried over MgSO4, filtered and concentrated to give 8.1 g (94.2%) of title compound as an orange solid foam.

1. customat ambient temperature
2. customovernight
3. concentrationThe dark orange solution is concentrated under reduced pressure (1-2 mm, <50° C.) to an orange oily residue
4. dissolutionThis oil is dissolved in 400 mL of ethyl acetate
5. washwashed with 100 mL of 1 N HCl (2×), with 150 mL of water (2×), and 100 mL of brine
6. dry with materialThe organic layer is dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated