Dimethylformamide dimethyl acetal → HCID 131729361, compound

Participants

Reaction Conditions

Reaction Steps

To a suspension of (3aR,7S,7aS)-7-(4-amino-3-fluoro-5-iodo-benzyl)-3-(3-tert-butyl-benzyl)-5,5-dioxo-hexahydro-1-oxa-5lambda*6*-thia-3-aza-inden-2-one (2.0 g, 3.2 mmol) in toluene (20 mL) was added N,N-dimethylformamid-dimethylacetal (1.18 g, 9.6 mmol) and the reaction mixture was heated in the microwave oven for 0.5 h at 150° C. After evaporation the residue was purified by chromatography (CombiFlash, 40 g silica gel, hexane-EtOAc 10:1 to EtOAc) to yield the title compound as beige crystals: TLC (hexane-EtOAc 1:1) Rf=0.39; HPLC RtA=1.92 min; ESIMS [M+H]+=641; 1H NMR (400 MHz, CDCl3): δ 7.58 (d, 1H), 7.35 (m, 3H), 7.09 (d, 1H), 6.82 (dd, 1H), 4.54 (d, 1H), 4.33 (d, 1H), 3.83 (dt, 1H), 3.76 (t, 1H), 3.1 (m, 2H), 3.08 (s, 3H), 3.02 (s, 3H), 2.83 (t, 1H), 2.74 (dd, 1H), 2.58 (m, 2H), 1.31 (s, 9H).

Provenance & Evidence