Phosphorus pentachloride → Methyl 2-chloro-1,3-benzoxazole-5-carboxylate
反応式
[CH3:1][O:2][C:3]([C:5]1[CH:6]=[CH:7][C:8]2[O:12][C:11](=S)[NH:10][C:9]=2[CH:14]=1)=[O:4].P(Cl)(Cl)(Cl)(Cl)[Cl:16]>P(Cl)(Cl)(Cl)=O>[Cl:16][C:11]1[O:12][C:8]2[CH:7]=[CH:6][C:5]([C:3]([O:2][CH3:1])=[O:4])=[CH:14][C:9]=2[N:10]=1参加物
4
実験手順
In a round bottom flask equipped with a magnetic stirrer, nitrogen inlet, reflux condenser and drying tube were placed 5-methoxycarbonylbenzoxazolthione (5.2 g, 0.025 mole), phosphorus pentachloride (5.2 g, 0,025 mole), and phosphorus oxychloride (40 mL). The reaction mixture was heated by an oil bath at 95°-100° C. for 4 hours. The reaction mixture was allowed to cool to room temperature and filtered. The filtrate was distilled with a short path distillation apparatus and the product was collected at 160°-163° C. at 29 mm Hg. The product solidified on standing to give a pale yellow solid, m.p. 104°-106° C. Anal Calcd. for C9H6ClNO3: C, 51.1; H, 2.9; N, 6.6; Cl, 16.8. Found: C, 50.7; H, 2.9; N, 6.6; Cl, 16.3