反应 #2336514

反应方程式

water

14

METHYL 4,6-DIBROMO-3-HYDROXYPYRIDINE-2-CARBOXYLATE

sodium hydride

benzyl chloride

→

15

收率 90.6%

METHYL 4,6-DIBROMO-3-BENZYLOXYPYRIDINE-2-CARBOXYLATE

收率 90.6%

溶剂

DMF

反应条件

后处理

1. 1
   workup.ADDITIONAfter the addition
2. 2
   温度The mixture was then heated at 90° C. for six hours
3. 3
   温度cooled
4. 4
   萃取extracted with ether (2×200 mL)
5. 5
   洗涤washed with 2N NaOH (50 mL)
6. 6
   干燥dried (MgSO4)
7. 7
   其他the solvent was evaporated

实验过程

To a stirred mixture of sodium hydride (0.6 g) in DMF (50 mL) was slowly added 14 (7.1 g). After the addition was complete, the mixture was stirred at room temperature for 15 minutes, then benzyl chloride (3.05 g) was added all at once. The mixture was then heated at 90° C. for six hours, cooled, poured into water (500 mL) and extracted with ether (2×200 mL). The ether extracts were combined, washed with 2N NaOH (50 mL), dried (MgSO4) and the solvent was evaporated to give 15 as a light yellow solid (8.3 g). Recrystallization from a small volume of methanol gave an analytical sample, m.p. 75-76° C.

来源