Hydrochloric Acid → Gsk-2981278

A solution of Super-Hydride® (1 M in tetrahydrofuran, 0.449 mL, 0.449 mmol) was added over 5 minutes, to a solution of methyl 5-(N-(4-ethylphenyl)-N-isobutylsulfamoyl)-2-((tetrahydro-2H-pyran-4-yl)methoxy)benzoate (100 mg, 0.204 mmol) in tetrahydrofuran (THF) (2 mL) under nitrogen. The solution was stirred for 1 hour then was added to a 1:1 mixture of ammonium chloride solution and HCl (2 N, 10 mL). The mixture was extracted with tert-butyl methyl ether (TBME) (2×5 mL), then organics dried and evaporated. The residue was purified by silica (Si) chromatography (0-50% ethyl acetate-cyclohexane) to give the title compound as a white foam (75 mg). LCMS [LCMS1] Rt 1.28 min, m/z (ES+) 462 (M+H).

1. extractionThe mixture was extracted with tert-butyl methyl ether (TBME) (2×5 mL)
2. customorganics dried
3. customevaporated
4. customThe residue was purified by silica (Si) chromatography (0-50% ethyl acetate-cyclohexane)

ORD-Eintrag

ord-badafb207efb4945b99776235ba544ba

Quelldatensatz

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09428452B2