Dichloromethane → HCID 9884191, compound

Participants

Reaction Steps

A mixture of the final product of Example 28 (150 mg) and [2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (Lawesson's Reagent) (189 mg) in 1,4-dioxane (5 mL) is heated at reflux for 1.5 hours and stirred at ambient temperature. After 18 hours, TLC analysis (5% CH3 0H--CH2Cl2) indicated the reaction to be complete. The mixture is diluted with water (50 mL), extracted with EtOAc (3×25 mL), dried over Na2SO4, filtered and concentrated under reduced pressure to a light yellow solid. The crude material is recrystallized from 5%CH3OH/EtOAc to give 119 mg of the title compound as a white solid, mp 238-240° C. dec and MS(ES) 337 (M+H)+ [α]25D.

Provenance & Evidence