Hydrochloric Acid → HCID 59486236, compound

Participants

Reaction Steps

HCl (91 mL, 360 mmol, 8 equiv, 4N in dioxane) is added dropwise to a cooled (10° C.) solution of (2-chloro-3,5-dimethoxy-6-methyl-phenyl)-carbamic acid tert-butyl ester (13.8 g, 45.7 mmol) in dioxane (150 mL), under an argon atmosphere. The reaction mixture is allowed to warm to RT, stirred for 24 h and concentrated. The residue is diluted with EtOAc, washed with a saturated aqueous solution of NaHCO3, and brine, dried (Na2SO4), filtered and concentrated. The residue is purified by crystallization from DCM/Hex to afford the title compound. ESI-MS: 202.0 [MH]+, TLC: Rf=0.37 (DCM).

Provenance & Evidence