反应详情

2-Amino-5-chlorobenzamide (Avocado)(1.00 g, 5.86 mmol, 1.0 eq.) and ethyl trifluoroacetate (4.19 mL, 35.2 mmol, 6.0 eq.) were dissolved in 50 mL of ethanol at rt under nitrogen and followed by the addition of 3.09 M sodium ethoxide in ethanol (11.38 mL, 35.2 mmol, 6.0 eq.) The mixture was refluxed 20 hours. Cooled to rt. Added 10 mL of 10% HOAc/H2O. Solids formed which were filtered, rinsed with 5 mL H2O, then dissolved in 20 mL of EtOAc/THF. Dried and stripped in vacuo to give 1.35 g of amber solids. LCMS detects (M+H)+=249.

1. temperaturewas refluxed 20 hours
2. customSolids formed which
3. filtrationwere filtered
4. washrinsed with 5 mL H2O
5. dissolutiondissolved in 20 mL of EtOAc/THF
6. customDried