Hydrochloric Acid → HCID 20295056, compound

Temperature

25 °C

Concentrated hydrochloric acid (1.0 ml) was added to a stirred suspension of 3,4-dichlorobenzaldehyde (140 g) in a mixture of trimethyl orthoformate (94 g) and dry methanol (400 ml). After stirring for 24 hours at laboratory temperature (about 25° C.), the reaction solution was adjusted to pH 7-8 by the addition of a solution of sodium methoxide in methanol and concentrated on a rotary evaporator. The residual oil was then dissolved in diethyl ether (600 ml). The ethereal solution was washed with water until the washings were neutral and then dried over anhydrous sodium sulphate, filtered and distilled to give 3,4-dichlorobenzaldehyde dimethyl acetal (157.5 g). b.p. 137°-140° C./25 mm Hg, as a clear mobile oil.

1. concentrationconcentrated on a rotary evaporator
2. dissolutionThe residual oil was then dissolved in diethyl ether (600 ml)
3. washThe ethereal solution was washed with water until the washings
4. dry with materialdried over anhydrous sodium sulphate
5. filtrationfiltered
6. distillationdistilled

ORD record

ord-b6ed1ee806b84bd0a54cfe245ce6bbce

Source dataset

uspto-grants-1981_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04246021