Hydrochloric Acid → HCID 58071511, compound

Participants

Reaction Conditions

Reaction Steps

Diethyl 1-(3-methoxy-4-nitrophenyl)phosphinane-4,4-dicarboxylate 1-oxide (INTERMEDIATE 59) (4.5 g, 10.89 mmol) and lithium hydroxide (1.043 g, 43.55 mmol) were added to a 200-mL round bottomed flask. Water (30 mL) and THF (30 mL) were added to give a brown suspension. The mixture was heated to 75° C. and stirred at that temperature for 4 h. The reaction mixture was concentrated to give a solid residue. To the mixture was added HCl (aq., 4 N, 60 mL) to give a suspension and further diluted with THF (30.0 mL). The mixture was microwaved at 110° C. for 2 h. After cooling to RT, water (60 mL) was added to the reaction solution. The solution was extracted with 30% iPrOH in chloroform (5×40 mL), and the combined organic layers were concentrated to give the title compound (0.4 g, 12% yield). m/z 314.

Provenance & Evidence