Trimethylphosphine → HCID 58668698, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 7-(3-Fluorobenzene-sulfonyl)-chroman-4-ol (3.0 g, 9.7 mmol) in THF (40 ml) and toluene (40 ml) was added HC(COOEt)3 (4.5 g, 19.5 mmol) and then PMe3 (19.5 ml of 1.0M THF solution). The mixture was cooled to −78° C. DIAD (4.0 g, 19.5 mmol) was added dropwise. The mixture was stirred at −78° C. for 1 hour and then at RT for overnight. The next day the TLC showed that the reaction was complete. The solvent was removed and the residue was partitioned between EtOAc and H2O. The EtOAc layer was washed with brine, dried with MgSO4, concentrated and purified with flash column to give 2-Ethoxycarbonyl-2-[7-(3-fluoro-benzenesulfonyl)-chroman-4-yl]-malonicacid diethyl ester: 5.0 g, clear oil. MS: 545 (M+Na)+.

Provenance & Evidence