Sodium thiocyanate → HCID 86650854, compound

17.91 g (120.5 mmol) of 3-chloro-5-methylhexan-2-one were dissolved in 120 ml of methyl ethyl ketone, 10.0 g (123.4 mmol) of sodium thiocyanate were added and the reaction mixture was heated under reflux for 1 h. After cooling, the reaction mixture was filtered, the residue was washed with methyl ethyl ketone and the combined filtrates were concentrated on a rotary evaporator. The oily residue was taken up in about 400 ml of dichloromethane and washed three times with in each case 100 ml of water. The organic phase was dried over sodium sulfate and the solvent was removed on a rotary evaporator. This gave 20.07 g of the crude product, which was reacted further as such.

1. temperaturethe reaction mixture was heated
2. temperatureunder reflux for 1 h
3. temperatureAfter cooling
4. filtrationthe reaction mixture was filtered
5. washthe residue was washed with methyl ethyl ketone
6. concentrationthe combined filtrates were concentrated on a rotary evaporator
7. washwashed three times with in each case 100 ml of water
8. dry with materialThe organic phase was dried over sodium sulfate
9. customthe solvent was removed on a rotary evaporator
10. customThis gave 20.07 g of the crude product, which was reacted further as such

ORD record

ord-90842205ff9044d2b899fb33ca4fe364

Source dataset

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08987256B2