反应详情

To a dichloromethane (25 mL) solution of amino-2-propyne (0.96 g, 17.43 mmol) and triethylamine (3.33 mL, 23.7 mmol) at 0° C. was added 3-phenoxybenzoyl chloride (3.68 g, 15.8 mmol) in dichloromethane (25 mL) in a dropwise fashion. The reaction was stirred for 1 h after removing the cooling bath and partitioned between dichloromethane and 10% aqueous HCl. The layers were separated and the aqueous layer was extracted with dichloromethane (2×). The combined organic layers were washed (1×, saturated sodium bicarbonate; 1×, brine), dried (MgSO4), and concentrated under vacuum to give a golden oil. Recrystallization with ehter ethyl acetate provided the title compound as a colorless solid (2.95 g, 74%).

1. customafter removing the cooling bath
2. custompartitioned between dichloromethane and 10% aqueous HCl
3. customThe layers were separated
4. extractionthe aqueous layer was extracted with dichloromethane (2×)
5. washThe combined organic layers were washed (1×, saturated sodium bicarbonate; 1×, brine)
6. dry with materialdried (MgSO4)
7. concentrationconcentrated under vacuum
8. customto give a golden oil
9. customRecrystallization with ehter ethyl acetate