Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate → HCID 19759865, compound

Participants

Reaction Steps

A solution of 2-allyl-2,3-dihydrothieno[2,3-b]thiophene-2-carboxylic acid-1,1-dioxide (8 g, 0.031 mol) and BOP reagent (17.8 g, 0.041 mol) in degassed DMF (150 mL) was cooled to 0° C. under nitrogen. Ethylamine was bubbled into the stirred reaction mixture until the solution was quite basic. After 1.5 hours, the DMF was removed in vacuo and the residue partitioned between ethyl acetate and 6N HCl. The aqueous phase was extracted a total of four times with ethyl acetate and the combined extracts washed with saturated sodium bicarbonate, brine, then dried over magnesium sulfate. Filtration and solvent removal gave the title compound as an oil (7.2 g).

Provenance & Evidence