반응 #217907

ord-ac9f9a605430414ea11139c1849030e1

반응 방정식

Cc1cc(C=O)ccc1O
4-hydroxy-3-methylbenzaldehyde
O=C([O-])[O-].[K+].[K+]
K2CO3
NC(=O)c1ccc(Cl)nc1
6-chloronicotinamide
O
H2O
[NH4+].[OH-]
NH4OH
수율 0.7%
Cc1cc(C=O)ccc1Oc1ccc(C(N)=O)cn1
title compound
Cc1cc(C=O)ccc1Oc1ccc(C(N)=O)cn1
6-(4-Formyl-2-methyl-phenoxy)-nicotinamide

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타irradiated for 5 min
  2. 2
    기타Upon completion of the reaction
  3. 3
    온도the mixture was cooled
  4. 4
    추출extracted with ethyl acetate
  5. 5
    세척the combined organic layers were washed twice with water and brine
  6. 6
    기타After drying the extracts
  7. 7
    기타over magnesium sulfate and evaporation under vacuum the crude product
  8. 8
    기타was purified by silica gel chromatography

실험 절차

A solution of 4-hydroxy-3-methylbenzaldehyde (1.0 equiv) in DMF (0.2 M solution) was treated with K2CO3 (1.5 equiv) and 6-chloronicotinamide (1.0 equiv). The reaction mixture was placed inside the microwave oven and then irradiated for 5 min. Upon completion of the reaction, the mixture was cooled, poured into H2O and extracted with ethyl acetate, and the combined organic layers were washed twice with water and brine. After drying the extracts over magnesium sulfate and evaporation under vacuum the crude product was purified by silica gel chromatography using CHCl3: EtOH 7%: NH4OH 0.7% to afford the title compound as a solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07381719B2uspto-grants-2008_06