ethyl 3-(1-benzofuran-2-yl)-3-oxopropanoate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 232 g of compound 3 are dissolved in 500 ml of ethanol. Cool in ice-bath and add 100 g of sodium borohydride in 500 ml of water. Stir for 2 hours. Add acetic acid until the sodium borohydride has been neutralized. Cool the solution in ice-bath under an atmosphere of nitrogen and add 10 g of 10% Pd/C catalyst. Stir under a hydrogen atmosphere at 15PSI until the reaction is complete, as judged by TLC. Filter through celite and evaporate organic solvents. Extract with ethyl acetate. Dry over sodium sulfate. Filter. Evaporate solvent. Cool in ice-bath Cool the solution in ice-bath under an atmosphere of nitrogen Stir under a hydrogen atmosphere at 15PSI until the reaction Filter through celite evaporate organic solvents Extract with ethyl acetate Dry over sodium sulfate Filter

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 122 g of salicylaldehyde 1 and 350 g of potassium carbonate are dissolved in 2L of acetone. While stirring at room temperature, add slowly 165 g of ethyl 4-chloroacetoacetate 2 over a period of 2 hours. When addition is over, stir at reflux for another 4 hours. Cool to room temperature and filter. Wash the filtration cake with 0.5L of acetone. Evaporate the solvent. When addition stir at reflux for another 4 hours Cool to room temperature filter Wash the filtration cake with 0.5L of acetone Evaporate the solvent

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 122 g of salicylaldehyde 1 and 350 g of potassium carbonate are dissolved in 2L of acetone. While stirring at room temperature, add slowly 165 g of ethyl 4-chloroacetoacetate 2 over a period of 2 hours. When addition is over, stir at reflux for another 4 hours. Cool to room temperature and filter. Wash the filtration cake with 0.5L of acetone. Evaporate the solvent. When addition stir at reflux for another 4 hours Cool to room temperature filter Wash the filtration cake with 0.5L of acetone Evaporate the solvent

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 232 g of compound 3 are dissolved in 500 ml of ethanol. Cool in ice-bath and add 100 g of sodium borohydride in 500 ml of water. Stir for 2 hours. Add acetic acid until the sodium borohydride has been neutralized. Cool the solution in ice-bath under an atmosphere of nitrogen and add 10 g of 10% Pd/C catalyst. Stir under a hydrogen atmosphere at 15PSI until the reaction is complete, as judged by TLC. Filter through celite and evaporate organic solvents. Extract with ethyl acetate. Dry over sodium sulfate. Filter. Evaporate solvent. Cool in ice-bath Cool the solution in ice-bath under an atmosphere of nitrogen Stir under a hydrogen atmosphere at 15PSI until the reaction Filter through celite evaporate organic solvents Extract with ethyl acetate Dry over sodium sulfate Filter

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 122 g of salicylaldehyde 1 and 350 g of potassium carbonate are dissolved in 2L of acetone. While stirring at room temperature, add slowly 165 g of ethyl 4-chloroacetoacetate 2 over a period of 2 hours. When addition is over, stir at reflux for another 4 hours. Cool to room temperature and filter. Wash the filtration cake with 0.5L of acetone. Evaporate the solvent. When addition stir at reflux for another 4 hours Cool to room temperature filter Wash the filtration cake with 0.5L of acetone Evaporate the solvent