Hydroxyamine hydrochloride → HCID 73865530, compound

A mixture of 6-(3-bromo-phenyl)-piperidine-2,5-dione (38.2 g) and hydroxylamine hydrochloride (19.8 g) in pyridine (300 ml) was stirred at room temperature under nitrogen. After 4 h the mixture was evaporated in vacuo. The crude mixture was partitioned between chloroform (200 ml) and water (200 ml) then was basified by the addition of 8% sodium bicarbonate solution (~300 ml). The mixture was extracted with chloroform (300 ml×2). The combined organic extracts were washed with saturated brine and evaporated in vacuo. Trituration with ether gave the title compound as a pale yellow solid (34.9 g). T.l.c. (Ethyl acetate) Rf 0.44, 0.28, E/Z mixture.

1. customAfter 4 h the mixture was evaporated in vacuo
2. customThe crude mixture was partitioned between chloroform (200 ml) and water (200 ml)
3. additionthen was basified by the addition of 8% sodium bicarbonate solution (~300 ml)
4. extractionThe mixture was extracted with chloroform (300 ml×2)
5. washThe combined organic extracts were washed with saturated brine
6. customevaporated in vacuo

ORD record

ord-2ddfd741547f4d34a6598437fc1b3de9

Source dataset

uspto-grants-1997_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05703240