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)-isoxazol-3-yl]-ethanol (110 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-6bf20a55beb241c79821c8b2e059208d

Quelldatensatz

uspto-grants-2008_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07456200B2