1-Chloroethyl chloroformate → HCID 58042836, compound

Participants

Reaction Steps

To 1.10 g (2.18 mmol) 4-benzyloxy-1-{2-[5-(2-chloro-benzyl)-4,5,6,7-tetrahydro-thieno[3,2-c]pyridin-2-yl]-2-oxo-ethyl}-1H-pyridin-2-one (example 38.1a) in 20 mL DCM is added at 0° C. 0.29 mL (2.61 mL) chloro-formic acid 1-chloro-ethyl ester. The reaction mixture is stirred 60 h at RT. Additional 0.29 mL (2.61 mL) chloro-formic acid 1-chloro-ethyl ester is added and the mixture is stirred overnight. Additional 0.29 mL (2.61 mL) chloro-formic acid 1-chloro-ethyl ester is added and the reaction mixture is refluxed overnight. The solvent is removed, to the residue 30 mL of methanol are added and the reaction mixture is refluxed for 30 min. After cooling to RT, the precipitate is collected after cooling the mixture to RT, washed with cold methanol and dried.

Provenance & Evidence