Ethyl cyanoacetate → HCID 69779882, compound

Participants

Reaction Steps

The title compound was prepared via the isocyanate from (5-amino-2-iodo-4-nitro-phenyl)-acetonitrile [prepared from 5-chloro-2-nitro-phenylamine by: i.) iodination with ICl/NaOAc in HOAc at 60° C.; ii.) reaction with ethyl cyanoacetate and KOBut in DMSO at 100° C. for 2 h.; iii.) deacarboxylation with LiCl/H2O in DMSO at 120° C. for 2.5 h] (5.15 g, 17 mmol) and diphosgene (2.05 mL, 17 mmol) in EtOAc (150 mL), followed by treatment with tert.-BuOH (25 mL) in CH2Cl2 (25 mL) according to the general procedure A (method a). Obtained as a yellow solid (4.00 g).

Provenance & Evidence