Triethylamine → HCID 18916377, compound

Participants

Reaction Steps

5.5 g (25 mmol) of methyl 3-(2-thienyl)-3-fluoro-2-hydroxybutyrate (Compound 1.1) are dissolved in 50 ml of dichloromethane, 3 g (30 mmol) of triethylamine are added, and 3.2 g (28 mmol) of methanesulfonyl chloride are added dropwise with stirring. The mixture is stirred for 2 hours at room temperature, washed with water, dried over magnesium sulfate and concentrated in vacuo. The residue is taken up in dimethylformamide (DMF), and this is added dropwise at 0° C. to a suspension of 12.9 g (75 mmol) of 4,6-dimethoxypyrimidine-2-thiol and 8.4 g (100 mmol) of sodium hydrogen carbonate in 100 ml of DMF. After the mixture has been stirred for 2 hours at room temperature and for a further 2 hours at 60° C., the mixture is poured into 1 l of ice-water, and the precipitate which has formed is filtered off with suction. After drying, 2.5 g of a white powder remain.

Provenance & Evidence