تفاعل #78091

معادلة التفاعل

3-(3-nitrophenyl)pyridine

dimethyl sulfate

dimethyl sulfate

→

1-methyl-3-(3-nitrophenyl)pyridinium methyl sulfate

المردود 82.0%

المذيبات

diethyl ether

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added (2×50 ml)
2. 2
   workup.ADDITIONwas added
3. 3
   ترشيحThe precipitate was filtered off
4. 4
   غسيلwashed several times with diethyl ether
5. 5
   workup.STIRRINGFinally, the precipitate was stirred in pyridine (100 ml) at 45° C. for 30 min
6. 6
   workup.ADDITIONTHF (250 ml) was added
7. 7
   workup.STIRRINGStirring
8. 8
   workup.WAITwas continued for additionally 30 min whereafter the product
9. 9
   ترشيحwas filtered off
10. 10
    غسيلwashed with diethyl ether
11. 11
    أخرىdried

الإجراء التجريبي

3-(3-nitrophenyl)pyridine (50 g, 0.25 mol) was added portion-wise with stirring to dimethyl sulfate (125 ml). The mixture was stirred at ambient temperature for 24 hours, during which time additional dimethyl sulfate was added (2×50 ml). At the end of the reaction diethyl ether (400 ml) was added, and the mixture was stirred in the cold for 2 hours. The precipitate was filtered off and washed several times with diethyl ether. Finally, the precipitate was stirred in pyridine (100 ml) at 45° C. for 30 min. THF (250 ml) was added. Stirring was continued for additionally 30 min whereafter the product was filtered off, washed with diethyl ether and dried to yield 1-methyl-3-(3-nitrophenyl)pyridinium methyl sulfate (66.6 g, 82%).

المصدر