تفاعل #2336514

معادلة التفاعل

water

14

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

sodium hydride

benzyl chloride

→

15

المردود 90.6%

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

المردود 90.6%

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONAfter the addition
2. 2
   درجة الحرارةThe mixture was then heated at 90° C. for six hours
3. 3
   درجة الحرارةcooled
4. 4
   استخلاصextracted with ether (2×200 mL)
5. 5
   غسيلwashed with 2N NaOH (50 mL)
6. 6
   تجفيفdried (MgSO4)
7. 7
   أخرىthe solvent was evaporated

الإجراء التجريبي

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.

المصدر