反应详情

Phosgene solution (1.75-M in toluene, 24 mmol) was added at 0° C. to a solution of compound (1) (20 mmol) in CH2Cl2 (40 mL). The reaction mixture was stirred at room temperature for 90 min, concentrated in vacuo, then redissolved in CH2Cl2 (40 mL) and treated with allylamine (42 mmol) at 0° C. The reaction was stirred for 4 h at room temperature, then water (40 mL) was added and the layers were separated. The aqueous layer was extracted with further CH2Cl2 (2×40 mL). The organic layers were washed with dilute HCl (20 mmol) and brine, dried (MgSO4) and concentrated in vacuo. The residue was triturated using diethyl ether to give the product (2) as a crystalline solid (3.5 g, 60%), m.p. 110-111° C. Found: C, 59.84; H, 6.11; N, 9.98. C14H17ClN2O2 requires: C, 59.89; H, 9.6.10; N, 9.97%.

1. concentrationconcentrated in vacuo
2. dissolutionredissolved in CH2Cl2 (40 mL)
3. stirringThe reaction was stirred for 4 h at room temperature
4. customthe layers were separated
5. extractionThe aqueous layer was extracted with further CH2Cl2 (2×40 mL)
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo
8. customThe residue was triturated