Sodium hydride → HCID 22827700, compound

Participants

Reaction Steps

8.13 g (0.03 mol) N-(hydroxyacetyl)-N-(2,4-dimethylthien-3-yl)-alanine-methylester is added in portions to a slurry of 1.05 g (0.035 mol) sodium hydride (80% in mineral oil) in 50 ml dry dimethoxyethane with stirring at 10°-15° under a blanket of nitrogen. The mixture is stirred at room temperature for half an hour, and then are added 4.3 g (0.03 mol) dimethylsulphamic acid chloride. The mixture is stirred for 18 hours at 50°, then cooled to room temperature, filtered, concentrated in vacuo, the residue taken up in CHCl3, washed thoroughly with water, dried over MgSO4 and evaporated in vacuo to yield the title compound.

Provenance & Evidence