methyl 5-cyano-1H-pyrrole-2-carboxylate

Conditions: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 20% solution of TiCl3 (25 ml, 32 mmol) in water was added to a solution of methyl 5-cyano-1-hydroxy-1H-pyrrole-2-carboxylate (Intermediate 128, 2.55 g, 15 mmol) in MeOH. The reaction was heated to an external temperature of 70° C. for 3 hours. The reaction mixture was concentrated to remove MeOH and the residue was partitioned with EtOAc and water. The organic portion was dried with MgSO4 and concentrated to an orange oil. The reaction mixture was concentrated to remove MeOH the residue was partitioned with EtOAc and water The organic portion was dried with MgSO4 concentrated to an orange oil

Conditions: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 20% solution of TiCl3 (25 ml, 32 mmol) in water was added to a solution of methyl 5-cyano-1-hydroxy-1H-pyrrole-2-carboxylate (Intermediate 128, 2.55 g, 15 mmol) in MeOH. The reaction was heated to an external temperature of 70° C. for 3 hours. The reaction mixture was concentrated to remove MeOH and the residue was partitioned with EtOAc and water. The organic portion was dried with MgSO4 and concentrated to an orange oil. The reaction mixture was concentrated to remove MeOH the residue was partitioned with EtOAc and water The organic portion was dried with MgSO4 concentrated to an orange oil