Hydrochloric Acid → HCID 68991126, compound

Participants

Reaction Conditions

Reaction Steps

Diisopropylamine (9.4 g) was added to a solution of n-Butyllithium (1.6 M in hexane, 43.7 mL) in THF (67 mL) at −78° C. The mixture was stirred for 10 min at 0° C. and then cooled to −78° C. and a solution of 3-Methyl-5-trimethylsilanyl-thiophene-2-carboxylic acid (5.0 g) in THF (40 mL) was added. The mixture was stirred at −78° C. for 30 min and then paraformaldehyde (3.2 g) was added. After warming to room temperature water and ethyl acetate were added. The aqueous phase was slightly acidified with HCl (10%) and then extracted three time with ethyl acetate. The combined organic phases were dried over sodium sulfate and the solvent was removed in vacuum. The raw product was purified by preparative HPLC. In this way the product was obtained with molecular weight 244.39 (C10H16O3SSi); MS (ESI): 245 (M+H+).

Provenance & Evidence