Isobutyryl chloride → HCID 12214103, compound

Participants

Reaction Steps

Ethyl isocyanoacetate (4.52 g) was added drop-wise to a stirred suspension of KOtBu in THF (35 ml) at 0° C. under nitrogen. After complete addition, the dark brown solution was stirred for 30 minutes and then a solution of isobutyryl chloride (2.1 ml) in THF (15 ml) added drop-wise, keeping the temperature below ˜10° C. The reaction was stirred for 1 hour then evaporated to dryness. The residue was treated with acetic acid (1.14 ml) and water (25 ml), and then extracted with ether (3×30 ml). The combined ether extracts were washed with saturated brine, dried over sodium sulfate, filtered and evaporated to give a brown oil that was purified by column chromatography, eluting with 1% MeOH in dichloromethane. This gave the title compound (1.91 g) as a colourless oil.

Provenance & Evidence