Ammonium Chloride → HCID 86744482, compound

Temperature

0 °C

To a slurry of 6.3 g of cuprous iodide in 70 ml of diethylether at 0° C. was added 44 ml of 1.5M methyllithium in ether over 15 minutes. The resulting solution was stirred for 20 minutes at 0° C., then cooled to -78° C. A solution of 6-chlorobicyclo[4.2.0]oct-2-en-7-one oxime, prepared as shown in Preparation 18, in ether was added and the mixture stirred at -78° C. to -60° C. for 30 minutes. Saturated ammonium chloride solution (10 ml) was slowly added and the mixture filtered. The filtrate was washed with ether, the combined washings dried over anhydrous sodium sulfate and solvent removed from the filtrate under reduced pressure, to give 6-methylbicyclo[4 2.0]oct-2-en-7-one oxime, the compound of formula (7A) where Y is hydrogen, 5.4 g.

1. temperaturecooled to -78° C
2. additionwas added
3. stirringthe mixture stirred at -78° C. to -60° C. for 30 minutes
4. filtrationthe mixture filtered
5. washThe filtrate was washed with ether
6. dry with materialthe combined washings dried over anhydrous sodium sulfate and solvent
7. customremoved from the filtrate under reduced pressure

ORD record

ord-d094c86f14b348b8b6b3d6fdc0775bc9

Source dataset

uspto-grants-1991_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04983627