Tetrahydrofuran → HCID 86642701, compound

Participants

Reaction Conditions

Reaction Steps

To a 100 mL round bottomed flask was added 4-methyl-4-nitropentyl iodide (2.0 g, 7.78 mmol), 2-butanone (20 mL) and a 1 M solution of trimethylphosphine in THF (15.5 mL, 2 equiv, 15.5 mmol). This flask was placed into a stainless steel pressure vessel, sealed and heated at 100° C. for 4 days. The vessel was cooled and opened in a fumehood. The flask was removed and contained a white solid. The steel vessel contained solvent. The white solid was suspended in ethyl acetate (100 mL), filtered, rinsed with EA (2×50 mL) and dried under high vacuum to give a pale yellow solid (2.39 g, 93%). 1H NMR (D2O, 400 MHz): δ 1.62 (s, 6H), 1.84-1.88 (d, J=14.4, 9H), 2.10-2.14 (m, 2H), 2.20-2.28 (m, 2H). LRMS (ESI+) for C9H21NO2P+ (206.1); Found: 206 (M+).

Provenance & Evidence