3,5-Dichlorobenzaldehyde → HCID 2741423, compound

80 ml of ethanol were added to 23.82 g (342.8 mmol) of hydroxylamine hydrochloride. After addition of 28.12 g (342.8 mmol) of sodium acetate, a solution of 50.00 g (285.7 mmol) of 3,5-dichlorobenzaldehyde in 100 ml ethanol was added dropwise within a period of 30 min, the mixture was stirred for 2 h and then allowed to stand overnight. The reaction mixture was concentrated to dryness, 500 ml of CH2Cl2 were then added and the mixture was washed with 400 ml of water. The aqueous phase was washed once with 100 ml of CH2Cl2, the organic phase was dried over Na2SO4, filtered off and concentrated. The residue was used without further purification. Yield: 56.50 g (98%)

1. waitto stand overnight
2. concentrationThe reaction mixture was concentrated to dryness, 500 ml of CH2Cl2
3. additionwere then added
4. washthe mixture was washed with 400 ml of water
5. washThe aqueous phase was washed once with 100 ml of CH2Cl2
6. dry with materialthe organic phase was dried over Na2SO4
7. filtrationfiltered off
8. concentrationconcentrated
9. customThe residue was used without further purification

ORD record

ord-b45167ace0704752b5a1cfe90cccf4f8

Source dataset

uspto-grants-2015_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09078442B2