تفاعل #2045108

معادلة التفاعل

1-methyl-2-trichloroacetyl-1H-pyrrole

nitric acid

→

1-Methyl-4-nitro-2-trichloroacetyl-1H-pyrrole

المذيبات

acetic anhydride

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture is slowly warmed to RT
2. 2
   workup.STIRRINGstirred vigorously for 2.5 h (initially oily deposit
3. 3
   أخرىcrystallization)
4. 4
   ترشيحThe precipitate is filtered off with suction
5. 5
   أخرىtriturated with 20 ml of methanol
6. 6
   ترشيحfiltered
7. 7
   أخرىdried under reduced pressure overnight
8. 8
   أخرىTo remove the regioisomers, which
9. 9
   أخرىare also formed
10. 10
    أخرىthe product is triturated with 10 ml of acetic acid/water 1:1 for 2 h
11. 11
    ترشيحthe solid is filtered off with suction
12. 12
    أخرىdried under reduced pressure
13. 13
    أخرىThis gives a solid

الإجراء التجريبي

2.12 g (9.34 mmol) of 1-methyl-2-trichloroacetyl-1H-pyrrole are dissolved in 9.5 ml of acetic anhydride and cooled to −20° C., and 0.43 ml (9.34 mmol) of nitric acid is added. The mixture is slowly warmed to RT and stirred at RT for 1 h. The reaction mixture is poured into 95 g of ice and stirred vigorously for 2.5 h (initially oily deposit then crystallization). The precipitate is filtered off with suction, triturated with 20 ml of methanol, filtered and dried under reduced pressure overnight. To remove the regioisomers, which are also formed, the product is triturated with 10 ml of acetic acid/water 1:1 for 2 h, and the solid is filtered off with suction and dried under reduced pressure. This gives a solid.

المصدر