Ammonium Chloride → HCID 86647903, Verbindung

Temperatur

-78 °C

To a vigorous stirring solution of tert-butyl (4-oxocyclohexyl)methylcarbamate (1.7 g) in tetrahydrofuran (40 mL) at −78° C. was dropwise added 1.6 M methyllithium (14.02 mL) in ether. After completion of the addition, the mixture was stirred at −78° C. for 1.2 hours and poured into a cold aqueous NH4Cl solution. The resulting mixture was extracted with dichloromethane (3×100 mL) and the organic layer was dried over Na2SO4, filtered and concentrated. The residue was dissolved in dichloromethane and loaded onto an Analogix purification system, eluted with 0-50% ethyl acetate in dichloromethane to provide the title compound.

1. customat −78° C.
2. additionAfter completion of the addition
3. extractionThe resulting mixture was extracted with dichloromethane (3×100 mL)
4. dry with materialthe organic layer was dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. dissolutionThe residue was dissolved in dichloromethane
8. customloaded onto an Analogix purification system
9. washeluted with 0-50% ethyl acetate in dichloromethane

ORD-Eintrag

ord-cd0be9d2cc904e80a96154a16f570021

Quelldatensatz

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09029404B2