반응 #41786

반응 방정식

MeCl2

5

4-amino-3-nitrophenol

6

[4-(4-amino-3-nitrophenoxy)(2-pyridyl)]-N-methylcarboxamide

sodium carbonate

→

desired product 7

nitroaniline

용매

DME H2O

water

ethyl acetate

반응 조건

후처리

1. 1
   기타by bubbling argon through the solution for 10 minutes
2. 2
   기타the reaction was sealed
3. 3
   온도The reaction was cooled to RT
4. 4
   기타The organic layer was separated from the aqueous layer
5. 5
   세척The aqueous layer was washed once more with ethyl acetate
6. 6
   건조dried (Na2SO4)
7. 7
   농축concentrated under vacuum

실험 절차

A solution of 5 (1 eq), 6 (1 eq), and sodium carbonate (1.2 eq) in DME/H2O (3:1) was degassed by bubbling argon through the solution for 10 minutes. Pd(II)(dppf)Cl2.MeCl2 (0.1 eq) was added to the reaction solution and the reaction was sealed. The reaction was heated at 100° C. overnight. The reaction was cooled to RT and ethyl acetate and water were added. The organic layer was separated from the aqueous layer. The aqueous layer was washed once more with ethyl acetate. The organic layers were combined, dried (Na2SO4), and concentrated under vacuum to yield the desired product 7. MS: MH+=469

출처