Hydrochloric Acid → 5331-92-0

Temperature

50 °C

3,4-Dichlorobenzaldehyde (1 eq) and hydroxylamine.HCl (4 eq) were suspended in pyridine (10 vol) in a sealed tube. The reaction mixture was stirred at 50° C. overnight under an atmosphere of N2. The reaction mixture was concentrated in vacuo before the addition of EtOAc (10 vol) and 2M citric acid solution (5 vol). The organic layer was separated and washed with citric acid (2×5 vol) and saturated aqueous NaCl solution (5 vol). The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure to yield required 3,4-dichloro-benzaldehyde oxime.

1. concentrationThe reaction mixture was concentrated in vacuo before the addition of EtOAc (10 vol) and 2M citric acid solution (5 vol)
2. customThe organic layer was separated
3. washwashed with citric acid (2×5 vol) and saturated aqueous NaCl solution (5 vol)
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure

ORD record

ord-c883f4be66f6498f8bc0f58d3be0c6a9

Source dataset

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08691824B2