Hydrochloric Acid → HCID 9860514, compound

Participants

Reaction Steps

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%.

Provenance & Evidence