反应详情

To a mixture of 8.34 g (49.8 mmol) of 2-chloro-N-(2-hydroxyphenyl)acetamide (PREPARATION 4) and 0.75 g (5 mmol) of sodium iodide in 25 ml of DMSO were added 3.56 g (5.47 mmol) of sodium azide. A moderate exotherm ensued. After stirring for 30 min the reaction was partitioned between ethyl ether and saline. The organic layers were dried over magnesium surfate and concentrated. The crude product was chromatographed on silica gel (700 ml) eluting with ethyl acetate/hexane (5/95), the appropriate fractions are pooled and concentrated to give the title compound, NMR (CDCl3) 4.60, 7.39, 7.56, 7.76 δ.

1. customwas partitioned between ethyl ether and saline
2. dry with materialThe organic layers were dried over magnesium surfate
3. concentrationconcentrated
4. customThe crude product was chromatographed on silica gel (700 ml)
5. washeluting with ethyl acetate/hexane (5/95)
6. concentrationconcentrated