Dichloromethane → HCID 66895863, compound

Participants

Reaction Steps

To a solution of 1,1-dimethylethyl{[5-(2-aminoethyl)-2,3-dichlorophenyl]methyl}cyclopropylcarbamate (1 eq.) from the previous step in dichloromethane (0.07 M) was added sequentially at 0 Hunig's base (1.2 eq.) and methyl chloroformate. The resulting solution was then allowed to warm slowly to RT over 3 h. The crude reaction mixture was subsequently diluted with ether and washed sequentially with 1 N aq. NaOH, 1 N aq. HCl, water and brine. The ether extract was then dried over Na2SO4, filtered and the filtrate concentrated in vacuo. Purification of the crude product thus obtained by way of flash chromatography (SiO2, 19:1 (v/v) Hex:EtOAc→EtOAc) afforded the title compound as a pale yellow oil.

Provenance & Evidence