تفاعل #420248

معادلة التفاعل

sodium

methanol

2,4-dichloro-6-methylpyrimidine

methanol

water

→

4-Chloro-2-methoxy-6-methyl-pyrimidine

ظروف التفاعل

المعالجة

1. 1
   أخرىhad formed
2. 2
   workup.ADDITIONThis solution was added dropwise over two hours
3. 3
   درجة الحرارةunder cooling so that the temperature
4. 4
   أخرىremained below 10° C
5. 5
   workup.STIRRINGStirring
6. 6
   ترشيحthe mixture was filtered
7. 7
   أخرىthe filtrate was evaporated to dryness under reduced pressure
8. 8
   أخرىThe residue was purified by column chromatography (pre-packed silica column, gradient of heptane/ethyl acetate)
9. 9
   أخرى750 mg was obtained (4.75 mmol, 47%)

الإجراء التجريبي

To anhydrous methanol (10 ml) was added sodium (230 mg, 10 mmol) and the mixture was stirred under an argon atmosphere until a clear solution had formed. This solution was added dropwise over two hours with stirring to a solution of 2,4-dichloro-6-methylpyrimidine (1.79 g, 11 mmol) in anhydrous methanol (10 ml) under cooling so that the temperature remained below 10° C. Stirring was continued for 30 minutes, then water was added (2 ml), the mixture was filtered and the filtrate was evaporated to dryness under reduced pressure. The residue was purified by column chromatography (pre-packed silica column, gradient of heptane/ethyl acetate). 750 mg was obtained (4.75 mmol, 47%). MS (APCI) m/z=159.2 [M+H]+.

المصدر