Acetic Acid → HCID 69286184, compound

Temperature

85 °C

In a bottom round flask equipped with a mechanical stirrer, a dropping funnel and a reflux condenser were loaded 265 g (3.08 mol) of the diethyl ketone with 252 g of butylacetate as the solvent, 0.36 molar equivalents of anhydrous magnesium chloride and the aforementioned titanium catalytic solution containing 0.053 molar equivalents of the trichloropropoxytitanium complex. The resulting suspension was stirred vigorously and allowed to heat to 85° C. Then 2.1 molar equivalents of propionaldehyde were added dropwise over 2 h at 85° C. The reaction was continued for an additional hour and cooled to 40° C. The reaction mixture was hydrolyzed with a 10% aqueous acetic acid solution (500 g), decanted and washed with a 10% aqueous acetic acid solution (200 g) and 50 g of NaCl. The organic phase was then washed twice with a 20% aqueous potassium carbonate solution.

1. customIn a bottom round flask equipped with a mechanical stirrer, a dropping funnel and a reflux condenser
2. waitThe reaction was continued for an additional hour
3. temperaturecooled to 40° C
4. customdecanted
5. washwashed with a 10% aqueous acetic acid solution (200 g) and 50 g of NaCl
6. washThe organic phase was then washed twice with a 20% aqueous potassium carbonate solution

ORD record

ord-141c4467d4064d8fb43df1ab7a2edc86

Source dataset

uspto-grants-2007_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07279605B2