Sodium Hydroxide → HCID 13665150, compound

Participants

Reaction Steps

(2S,4S)-N-methanesulfonyl-4-dicyclohexylphosphinyl-2 -diphenylphosphinylmethylpyrrolidine [IX] in an amount of 350 mg was mixed with and dissolved in 700 mg of phenol and 5.3 ml of 48% hydrobromic acid, and the solution was refluxed in nitrogen atmosphere for 8-10 hours. After completion of the reaction, the solution was made alkaline with a 30% aqueous solution of caustic soda and was then extracted three times with 20 ml of ethyl acetate in each case. The extract was washed with 20 ml of water and then with 20 ml of a saturated solution of sodium chloride, dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by way of column chromatography on silica gel whereby 196 mg (yield: 65%) of the title compound was obtained as crystals.

Provenance & Evidence