Water → HCID 68844294, compound

Participants

Reaction Steps

To a solution of the product of Step 7 (8.50 g, 25.3 mmol) in tetrahydrofuran (85 mL) was added triphenylphosphine (6.65 g, 25.3 mmol) and H2O (0.91 g, 50.7 mmol). The solution was stirred at reflux for 3 hours and then cooled to room temperature and concentrated. The residue was dissolved in 4.0 N aqueous HCl (200 mL) and extracted with chloroform (200 mL). The aqueous layer was basified to pH 10 with concentrated aqueous ammonium hydroxide solution and the resulting mixture was extracted with chloroform (2×300 mL). The combined organic extracts were dried over sodium sulfate and concentrated to afford 7.84 g (99%) of the product as a solid. MS m/z 310.3 (AP+100).

Provenance & Evidence