Hydrochloric Acid → HCID 74061803, compound

30.00 g (157.9 mmol) of 3,5-dichlorobenzaldehyde oxime were initially charged in ml of 0.5M HCl in DMF, and 116.7 g (189.5 mmol) of Oxone (potassium peroxomonosulfate) were added a little at a time at room temperature (RT). So that the internal temperature of the reaction mixture did not exceed 50° C., the mixture was cooled with an ice bath. After 2 h, the reaction solution was poured into 1 l of ice water and extracted twice with 500 ml of ether each time. The combined organic phases were then washed with 400 ml of 0.5M aqueous HCl and with 200 ml of saturated NaCl solution, dried over Na2SO4, filtered off and concentrated. The residue was used without further purification. Yield: 28.40 g (80%)

1. additionwere added a little at a time at room temperature (RT)
2. customdid not exceed 50° C.
3. temperaturethe mixture was cooled with an ice bath
4. extractionextracted twice with 500 ml of ether each time
5. washThe combined organic phases were then washed with 400 ml of 0.5M aqueous HCl and with 200 ml of saturated NaCl solution
6. dry with materialdried over Na2SO4
7. filtrationfiltered off
8. concentrationconcentrated
9. customThe residue was used without further purification

ORD record

ord-0c54488b836d4f1d89ec45e2d7d1d1e4

Source dataset

uspto-grants-2015_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09078442B2