Triethyl phosphite → HCID 15341134, compound

Participants

Reaction Steps

A solution containing 3,3'-bis(trifluoromethyl)benzhydryl bromide (29.8 g, 77.6 mmol), prepared according to methods in Example 3 and triethyl phosphite (21.6 mL, 126 mmol), was heated at 155°-160° C. for 16 hours, under N2. The reaction mixture was cooled and washed with H2O (2×150 mL) to remove the excess triethyl phosphite. The non-aqueous portion was added to CH2Cl2 (150 mL), dried (MgSO4), filtered, and concentrated in volume to give a pale yellow oil, 30.1 g. The crude product was chromatographed on a silica gel column. Elution with ethyl acetate/hexane (1:1) afforded analytically pure product as a white solid, 10.7 g, (31.2%), mp 82°-85° C. 300MHz 1H NMR (CDCl3): δ,4.54 (d,1H, J=25.3 Hz, PCH). MS: 441 (M+1).

Provenance & Evidence