HCID 58409382, compound → HCID 178448797, compound

Participants

Reaction Steps

The r indicates a number of repeat units of Ti(N(n-Bu)2. Reaction is set up in a glove box under N2 atmosphere. A 20-mL vial equipped with a stir bar is charged with (0.4858 g, 1.7900 mmol) of 2-(2,6-diisopropylphenylamino)cyclohex-2-enone (Preparation 3), toluene (6.0 mL) and (0.3022 g, 0.8984 mmol) of polymeric n-butylamino-titanium reagent (Preparation 4). The mixture is stirred overnight (24 hours). 1H-NMR of aliquot showed reaction is not complete. About 26% of starting material remained. Therefore, to the mixture are added 46.2 mg of polymeric n-butylamino-titanium reagent (Preparation 4). After stirring overnight, 1H-NMR of aliquot showed that no starting material remained. To the mixture are added hexanes, and the resulting mixture is filtered. Hexanes are also used to wash filtercake solids. The filtrate (yellow solution) is concentrated under reduced pressure to afford 305.8 mg (52.3%) of compound (B) of Example B as a yellow oil.

Provenance & Evidence