3-chloropropanamide

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: 6.42 g (60 mmol) 3-Chloropropanamide, 5.85 g (30 mmol) N-methyl-3,4-dimethoxybenzeneethanamine and 7.7 g (75 mmol) triethylamine in 100 ml acetonitrile were stirred under reflux for 18 hours. The reaction mixture was concentrated in vacuo and the residue purified by chromatography on silicagel using methylene chloride/methanol: 92/8 to yield 5.12 g (64.1%) of the desired compound as an orange oil. under reflux for 18 hours The reaction mixture was concentrated in vacuo the residue purified by chromatography on silicagel

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

実験手順: A mixture of 15.2 g (0.05 mole) of α,α-bis(4-fluorophenyl)-4-piperidinemethanol, 5.9 g (0.055 mole) of 3-chloropropionamide (Aldrich), 15.9 g (0.15 mole) of anhydrous sodium bicarbonate and 0.4 g of potassium iodide in 150 ml of dimethylformamide was heated on a steam bath for 24 h. The mixture was poured into 1.5 L of water and a solid precipitated. After standing overnight, the solid was collected by filtration, washed with water, dried, and recrystallized from benzene to yield 13.9 g (74%) of white solid, mp 136°-137° C. was heated on a steam bath for 24 h a solid precipitated the solid was collected by filtration washed with water dried recrystallized from benzene

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

実験手順: A mixture of 0.2 mole 3-chloropropionamide, 35 ml. of acetic anhydride and 1 ml. acetylchloride is refluxed under nitrogen for 1 hour and then concentrated in vacuo to give crude N-acetyl-3-chloropropionamide as an oil which is used in the next step without purification. concentrated in vacuo

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

実験手順: 6.42 g (60 mmol) 3-Chloropropanamide, 5.85 g (30 mmol) N-methyl-3,4-dimethoxybenzeneethanamine and 7.7 g (75 mmol) triethylamine in 100 ml acetonitrile were stirred under reflux for 18 hours. The reaction mixture was concentrated in vacuo and the residue purified by chromatography on silicagel using methylene chloride/methanol: 92/8 to yield 5.12 g (64.1%) of the desired compound as an orange oil. under reflux for 18 hours The reaction mixture was concentrated in vacuo the residue purified by chromatography on silicagel

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

実験手順: A mixture of 15.2 g (0.05 mole) of α,α-bis(4-fluorophenyl)-4-piperidinemethanol, 5.9 g (0.055 mole) of 3-chloropropionamide (Aldrich), 15.9 g (0.15 mole) of anhydrous sodium bicarbonate and 0.4 g of potassium iodide in 150 ml of dimethylformamide was heated on a steam bath for 24 h. The mixture was poured into 1.5 L of water and a solid precipitated. After standing overnight, the solid was collected by filtration, washed with water, dried, and recrystallized from benzene to yield 13.9 g (74%) of white solid, mp 136°-137° C. was heated on a steam bath for 24 h a solid precipitated the solid was collected by filtration washed with water dried recrystallized from benzene

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

実験手順: A mixture of 15.2 g (0.05 mole) of α,α-bis(4-fluorophenyl)-4-piperidinemethanol, 5.9 g (0.055 mole) of 3-chloropropionamide (Aldrich), 15.9 g (0.15 mole) of anhydrous sodium bicarbonate and 0.4 g of potassium iodide in 150 ml of dimethylformamide was heated on a steam bath for 24 h. The mixture was poured into 1.5 L of water and a solid precipitated. After standing overnight, the solid was collected by filtration, washed with water, dried, and recrystallized from benzene to yield 13.9 g (74%) of white solid, mp 136°-137° C. was heated on a steam bath for 24 h a solid precipitated the solid was collected by filtration washed with water dried recrystallized from benzene

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: A mixture of 0.2 mole 3-chloropropionamide, 35 ml. of acetic anhydride and 1 ml. acetylchloride is refluxed under nitrogen for 1 hour and then concentrated in vacuo to give crude N-acetyl-3-chloropropionamide as an oil which is used in the next step without purification. concentrated in vacuo

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

実験手順: 6.42 g (60 mmol) 3-Chloropropanamide, 5.85 g (30mmol) N-methyl-3,4-dimethoxybenzeneethanamine and 7.7 g (75 mmol) triethylamine in 100 ml acetonitrile were stirred under reflux for 18 hours. The reaction mixture was concentrated in vacuo and the residue purified by chromatography on silicagel using methylene chloride/methanol: 92/8 to yield 5.12 g (64.1%) of the desired compound as an orange oil. under reflux for 18 hours The reaction mixture was concentrated in vacuo the residue purified by chromatography on silicagel

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 2.7 g of α,2-dimethyl-5H-[1]benzopyrano [2,3-b]pyridine-7-acetic acid in 15 ml of dimethylformamide are added 0.8 g of potassium carbonate and 1.3 g of 3-chloropropionamide, and stirred at 70° C. for 7.5 hours under a nitrogen atmosphere. The reaction mixture is poured into ice water. The precipitate is extracted with ethyl acetate, washed with water and dried, and then concentrated. The residue is recrystallized from ethanol to obtain 2.4 g of 2-carbamoylethyl α,2-dimethyl-5H-[1]benzopyrano[2,3-b]pyridine7-acetate as white crystals having a melting point of 143° to 145° C. The precipitate is extracted with ethyl acetate washed with water dried concentrated The residue is recrystallized from ethanol

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

実験手順: A mixture of 0.2 mole 3-chloropropionamide, 35 ml. of acetic anhydride and 1 ml. acetylchloride is refluxed under nitrogen for 1 hour and then concentrated in vacuo to give crude N-acetyl-3-chloropropionamide as an oil which is used in the next step without purification. concentrated in vacuo