Sodium Sulfate → HCID 55285529, compound

An ethanol-water solution (1:3, 4 mL) of 3,4,4-trimethylcyclohex-2-enone (500 mg, 3.62 mmol) and sodium acetate (356 mg, 4.35 mmol) was stirred with hydroxylamine sulfate (475 mg, 2.89 mmol) at 70° C. for 40 hours. After completion of the reaction, the reaction solution was extracted with ethyl acetate, and the resulting organic layer was evaporated under reduced pressure. The resulting residue was dissolved in tetrahydrofuran (5 mL), mixed with lithium aluminum hydride (412 mg, 10.9 mmol) at 0° C. and stirred at room temperature for 2 hours. After completion of the reaction, the reaction solution was mixed with saturated aqueous sodium sulfate, dried over anhydrous magnesium sulfate and filtered through celite, and the solvent was removed by vacuum distillation to give the desired product.

1. customAfter completion of the reaction
2. extractionthe reaction solution was extracted with ethyl acetate
3. customthe resulting organic layer was evaporated under reduced pressure
4. dissolutionThe resulting residue was dissolved in tetrahydrofuran (5 mL)
5. customAfter completion of the reaction
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltered through celite
8. customthe solvent was removed by vacuum distillation

ORD record

ord-34427dba363f4743be671210b6a3bcc1

Source dataset

uspto-grants-2013_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08440666B2