反应 #1850

反应方程式

3-hydroxy-2-iodo-6-methylpyridine

potassium acetate

triphenylphosphine

ethyl acrylate

→

Ethyl (3-hydroxy-6-methylpyridin-2-yl)propenoate

溶剂

DMF

water

反应条件

后处理

1. 1
   温度The mixture was cooled
2. 2
   过滤filtered
3. 3
   workup.ADDITIONadded to water (100 ml)
4. 4
   萃取The product was extracted into ethyl acetate (3×30 ml)
5. 5
   洗涤The combined extracts were washed with water (2×25 ml) and with brine (25 ml)
6. 6
   干燥dried over sodium sulphate
7. 7
   其他evaporated
8. 8
   workup.WAITThis left a tan solid

实验过程

To a solution of 3-hydroxy-2-iodo-6-methylpyridine (1.175 g, 5.0 mmol) in DMF (9.5 ml) and water (0.5 ml) were added potassium acetate (1.23 g, 12.5 mmol), triphenylphosphine (105 mg, 0.40 mmol), palladium chloride (36 mg, 0.20 mmol) and ethyl acrylate (1.63 ml, 1.50 g, 15.0 mmol). The mixture was placed under nitrogen and heated at 120° C. for 1.5 h. The mixture was cooled, filtered from deposited palladium black, and added to water (100 ml). The product was extracted into ethyl acetate (3×30 ml). The combined extracts were washed with water (2×25 ml) and with brine (25 ml), then dried over sodium sulphate and evaporated. This left a tan solid, the product (951 mg, 91%). mp 192°-195° C. (dec)

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