反应详情

11 G. (0.05 moles) of 2-amino 5-iodo pyridine, 7.2 ml. (0.07 moles) of thiophenol, 3.8 g. (0.07 moles) of sodium methoxide, 1.0 g of copper powder and 100 ml. of methanol are heated 150° C. for 12 hours in a glass lined bomb. The reaction mixture is concentrated to dryness, extracted with chloroform and the chloroform extracts concentrated to dryness in vacuo affording 15 g. of a crude product which is chromatographed on 600 g. of silica gel, eluting with methylene chloride and ethyl acetate-methylene chloride 50% mixture affording 6.5 g of 2-amino 5-phenylthio pyridine, m.p. 127° to 129° C.

1. concentrationThe reaction mixture is concentrated to dryness
2. extractionextracted with chloroform
3. concentrationthe chloroform extracts concentrated to dryness in vacuo
4. customaffording 15 g
5. customof a crude product which is chromatographed on 600 g
6. washof silica gel, eluting with methylene chloride and ethyl acetate-methylene chloride 50% mixture