Ethanol → N-[(2R,6S)-2,6-Dimethylcyclohexylidene]hydroxylamine

5 g of 2,6-dimethylcyclohexanone and 5.51 g of hydroxylamine hydrochloride were suspended to 80 ml of ethanol, then 9.4 g of pyridine was dropped at 0° C. The mixture was stirred at room temperature for 4 hours, then the reaction mixture was concentrated. Water was added to the residue and extracted with ethyl acetate three times. The organic layers were joined, washed with saturated aqueous solution of sodium chloride, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 3.1 g of cis-2,6-dimethylcyclohexanoneoxime and 1.3 g of trans-2,6-dimethylcyclohexanoneoxime.

1. concentrationthe reaction mixture was concentrated
2. additionWater was added to the residue
3. extractionextracted with ethyl acetate three times
4. washwashed with saturated aqueous solution of sodium chloride
5. dry with materialdried with anhydrous magnesium sulfate
6. concentrationconcentrated

ORDレコード

ord-632e3ea77dfc479bbd2fd58a8a6cd439

出典データセット

uspto-grants-2012_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08101753B2