Dichloromethane → HCID 11604158, compound

Participants

Reaction Steps

A mixture of example 2 (11 mg), 1-chloroethyl chloridocarbonate (4 μL) and TEA (6.5 μL) in anhydrous 1,2-dichloroethane (100 μL) was refluxed under a Nitrogen atmosphere for 1 h. Additional 1-chloroethyl chloridocarbonate (3×4 μL) and TEA (3×6.5 μL) were added during the following 5 h while stirring. The mixture was concentrated under vacuum, MeOH (200 μL) was added to the residue and resulting mixture refluxed for 1 h. DCM and an aqueous std NaHCO3 solution were added to the crude residue and the aqueous phase extracted with DCM. The organic extracts were collected, dried and evaporated under vacuum to give a crude which was purified by flash cromathography (eluting with DCM:MeOH=95:5 to 9:1, then 8:2 containing 0.5% NH4OH) to afford the title compound (5.8 mg) as a off-white foam.

Provenance & Evidence