Toluene → HCID 13742722, compound

Participants

Reaction Steps

To a stirred soIution of ethyl 2-amino-thiophene-3-carboxylate (5,0 g, 29 mmol) and triethylamine (4,1 ml, 29 mmol) in dry tetrahydrofuran (100 ml) was added a 20% solution of phosgene in toluene (16 ml, 32 mmol). The mixture was heated to reflux for 3 h, then cooled to room temperature and exposed to a gaseous stream of methylamine for 10 min. After additional stirring for 30 min., the mixture was filtered and the filtrate was evaporated in vacuo, whereafter the crystalline residue was suspended in water, filtered off, and dried to give the title compound as colourless crystals, m.p. 127° C.

Provenance & Evidence