Diisopropylethylamine → HCID 86628361, compound

Participants

Reaction Steps

A mixture of 1,1-dimethylethyl (1-{2-[6-fluoro-3-(methyloxy)-5-quinoxalinyl]-3-hydroxypropyl}-4-piperidinyl)carbamate (10.8 g, 25 mmol), methanesulfonic anhydride (5.12 g, 28.7 mmol) and N,N-diisopropylethylamine (9.8 ml, 56 mmol) in dry chloroform (140 ml) was stirred at room temperature for 0.5 h, then heated under reflux for 3 days. The mixture was washed with aqueous sodium bicarbonate and the aqueous phase was extracted with dichloromethane. The combined organic fractions were dried and evaporated. The residue was chromatographed on silica (500 g), eluting with 0-5% methanol/dichloromethane to give the product (8.13 g, 81%).

Provenance & Evidence