Sodium Iodide → HCID 20273728, compound

Participants

Reaction Steps

A mixture of Intermediate 22 (5 g), triphenylphosphine (33.6 g), NaHCO3 (7 g) and NaI (19.3 g) in acetonitrile (175 ml) was heated under reflux for 17 h. After cooling the inorganic solids were filtered off and washed with dichloromethane. The combined filtrates were evaporated and the residue was triturated firstly with ER (discarded) and then with CH2Cl2. The CH2Cl2 extracts were evaporated in vacuo and the residue, which solidified on trituration with ER, was crystallised from EA-acetonitrile to give the title compound (8.1 g) m.p. 189°-191°.

Provenance & Evidence