2-ethylbut-1-enyl propanoate

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

実験手順: A reaction vessel was charged sequentially with Et3N (12.8 L), propionic anhydride (14.48 L), dimethylaminopyridine (94 gm) and 2-ethylbutyraldehyde (7.5 L). The mixture was stirred and heated under gentle reflux (120°-135° C.) for 5 hours in a nitrogen atmosphere. The reaction was then cooled to 70° C. and H2O (13.5 L) was added slowly. On complete addition, the mixture was heated at reflux for 45 minutes and then cooled to room temperature before hexane (7.5 L) was added. The aqueous layer was separated and re-extracted with hexane (5 L) and the combined organic layers were washed with saturated NaHCO3 (2×7.5 L) before being evaporated in vacuo at 40° C. The residue (10 Kg) so obtained was fractionally distilled (b.p. 75°-80° C., 30-40 mm Hg) to give the required product (7.712 Kg) as a mobile liquid. heated under gentle reflux (120°-135° C.) for 5 hours in a nitrogen atmosphere On complete addition the mixture was heated at reflux for 45 minutes was added The aqueous layer was separated re-extracted with hexane (5 L) the combined organic layers were washed with saturated NaHCO3 (2×7.5 L) before being evaporated in vacuo at 40° C

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

実験手順: A reaction vessel was charged sequentially with Et3N (12.8 L), propionic anhydride (14.48 L), dimethylaminopyridine (94 gm) and 2-ethylbutyraldehyde (7.5 L). The mixture was stirred and heated under gentle reflux (120°-135° C.) for 5 hours in a nitrogen atmosphere. The reaction was then cooled to 70° C. and H2O (13.5 L) was added slowly. On complete addition, the mixture was heated at reflux for 45 minutes and then cooled to room temperature before hexane (7.5 L) was added. The aqueous layer was separated and re-extracted with hexane (5 L) and the combined organic layers were washed with saturated NaHCO3 (2×7.5 L) before being evaporated in vacuo at 40° C. The residue (10 Kg) so obtained was fractionally distilled (b.p. 75°-80° C., 30-40 mm Hg) to give the required product (7.712 Kg) as a mobile liquid. heated under gentle reflux (120°-135° C.) for 5 hours in a nitrogen atmosphere On complete addition the mixture was heated at reflux for 45 minutes was added The aqueous layer was separated re-extracted with hexane (5 L) the combined organic layers were washed with saturated NaHCO3 (2×7.5 L) before being evaporated in vacuo at 40° C

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

実験手順: A reaction vessel was charged sequentially with Et3N (12.8 L), propionic anhydride (14.48 L), dimethylaminopyridine (94 gm) and 2-ethylbutyraldehyde (7.5 L). The mixture was stirred and heated under gentle reflux (120°-135° C.) for 5 hours in a nitrogen atmosphere. The reaction was then cooled to 70° C. and H2O (13.5 L) was added slowly. On complete addition, the mixture was heated at reflux for 45 minutes and then cooled to room temperature before hexane (7.5 L) was added. The aqueous layer was separated and re-extracted with hexane (5 L) and the combined organic layers were washed with saturated NaHCO3 (2×7.5 L) before being evaporated in vacuo at 40° C. The residue (10 Kg) so obtained was fractionally distilled (b.p. 75°-80° C., 30-40 mm Hg) to give the required product (7.712 Kg) as a mobile liquid. heated under gentle reflux (120°-135° C.) for 5 hours in a nitrogen atmosphere On complete addition the mixture was heated at reflux for 45 minutes was added The aqueous layer was separated re-extracted with hexane (5 L) the combined organic layers were washed with saturated NaHCO3 (2×7.5 L) before being evaporated in vacuo at 40° C