Sodium Carbonate → HCID 73516726, compound

A mixture of 20 gm (167 mMol) N,N-dimethyl-5-amino-2-pentanone, 14.5 gm (208 mMol) hydroxylamine hydrochloride, and 8.8 gm (83 mMol) sodium carbonate in 50 mL water was heated at reflux for 1.5 hours. After cooling to room temperature, the reaction mixture was extracted with dichloromethane. The organic extracts were combined, dried over sodium sulfate and concentrated under reduced pressure. The residual oil crystallized on standing at room temperature. The solid was washed with hexane to provide 12.8 gm (54%) of the desired oxime as a colorless solid in two crops.

1. temperaturewas heated
2. temperatureat reflux for 1.5 hours
3. extractionthe reaction mixture was extracted with dichloromethane
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residual oil crystallized
7. customon standing at room temperature
8. washThe solid was washed with hexane

ORD record

ord-1084d9d7dcad4f66b98cc1a27a1ebaac

Source dataset

uspto-grants-1998_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05792763