Hydrochloric Acid → HCID 13139214, compound

Temperature

0 °C

Thereafter, the mixture is heated under reflux for 1 hour and then cooled to 0° C. 60 g of 3-methylbenzaldehyde, dissolved in 250 ml of absolute ether, are added dropwise at 0° C. The reaction solution is left to stand overnight and is then poured onto 1 l of ice-water. The reaction mixture is acidified with 2N hydrochloric acid. The organic phase is separated off, the aqueous phase is extracted twice with 300 ml of ethyl acetate each time and the combined organic phases are washed twice with 200 ml of water each time, dried over MgSO4 and evaporated on a rotary evaporator in vacuo. The residue is distilled at 64°-66° C./0.02 mm.

1. temperatureThereafter, the mixture is heated
2. temperatureunder reflux for 1 hour
3. additionare added dropwise at 0° C
4. waitThe reaction solution is left
5. customThe organic phase is separated off
6. extractionthe aqueous phase is extracted twice with 300 ml of ethyl acetate each time
7. washthe combined organic phases are washed twice with 200 ml of water each time
8. dry with materialdried over MgSO4
9. customevaporated on a rotary evaporator in vacuo
10. distillationThe residue is distilled at 64°-66° C./0.02 mm

ORD record

ord-8528560b935f40eb8e8bf72f416ed672

Source dataset

uspto-grants-1991_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05006534