HCID 131733559, compound → HCID 131733560, compound

Participants

Reaction Steps

A solution of [(R)-1-hydroxymethyl-2-(3-iodo-phenyl)-ethyl]-carbamic acid tert-butyl ester K-9 (5.32 g, 14.1 mmol) in DCM (100 mL) was added dropwise to a RT suspension of DMP (6.78 g, 15.5 mmol) in DCM (40 mL) and the resulting mixture was stirred for 1.5 h. The reaction was quenched with 20% aq. NaHCO3 and 10% aq. Na2S2O3 and stirred for 1 h. The layers were separated and the aqueous layer was extracted with DCM (2×). The combined organic extracts were washed with 1M aq. HCl, brine, dried over Na2SO4, filtered and evaporated in vacuo. The crude product was subsequently triturated with a little DCM to give the title compound as an orange solid. LC-MS A: tR=0.87 min; [M+H]+=No ionisation.

Provenance & Evidence