Triethylamine → Methanesulfonic acid 1-[5-(3-Chloro-phenyl)-isoxazol-3-yl]-ethyl ester

Temperatur

0 °C

In a screw cap vial equipped with stir bar was added 1-[5-(3-chloro-phenyl)-isoxazole-3-yl]-ethanol (10 mg, 0.49 mmol), dichloromethane (3 ml) and triethylamine (0.34 ml, 2.46 mmol). Cooled the mixture down to 0° C. and to it added methane sulfonyl chloride (0.08 ml, 0.98 mmol). Left the reaction mixture stirring at room temperature for 30 min. Reaction was quenched with saturated sodium bicarbonate (aqueous, 40 ml) and extracted with dichloromethane (3×30 ml). Combined organic phase was washed with brine (40 ml), dried (sodium sulfate), filtered and concentrated, in-vacuo to isolate the desired compound as brown oil.

1. customIn a screw cap vial
2. customequipped
3. waitLeft the reaction mixture
4. stirringstirring at room temperature for 30 min
5. customReaction
6. customwas quenched with saturated sodium bicarbonate (aqueous, 40 ml)
7. extractionextracted with dichloromethane (3×30 ml)
8. washCombined organic phase was washed with brine (40 ml)
9. dry with materialdried (sodium sulfate)
10. filtrationfiltered
11. concentrationconcentrated

ORD-Eintrag

ord-1b966cefb1ac49b782b6b8ea6654dc62

Quelldatensatz

uspto-grants-2009_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07585881B2