HRID434465

反应详情

EQUATION

反应方程式

HRID 434465 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Chloro-3,5-dinitrobenzotrifluoride (5.4 grams; 0.02 mole) dissolved in benzene was charged into a glass reaction vessel equipped with a mechanical stirrer and addition funnel. N-Methyl-N-2,2-dimethoxyethylamine (2,4 grams; 0.02 mole) and triethylamine (2.02 grams; 0.02 mole) both dissolved in benzene (50 ml) were then added dropwise with stirring. After the addition was completed stirring was continued for a period of 1 hour resulting in the formation of a precipitate. The reaction mixture was filtered to remove the acid acceptor salt and was chromatographed. The solution was then evaporated to yield a solid product. This solid was recrystallized from hexane to yield the desired product N-methyl-N-(2,2-dimethoxyethyl)-2,6-dinitro-4-trifluoroemethylaniline melting at 48° to 50° C.

WORKUP

后处理

  1. additionwas charged into a glass reaction vessel
  2. customequipped with a mechanical stirrer and addition funnel
  3. additionwere then added dropwise
  4. additionAfter the addition
  5. stirringwas completed stirring
  6. customresulting in the formation of a precipitate
  7. filtrationThe reaction mixture was filtered
  8. customto remove the acid acceptor salt
  9. customwas chromatographed
  10. customThe solution was then evaporated
  11. customto yield a solid product
  12. customThis solid was recrystallized from hexane