Ethyl 2-methylacetoacetate → HCID 178432484, compound

Participants

Reaction Conditions

Reaction Steps

To 2-chlorobenzimidamide (34.07 g, 220 mmol) and triethylamine (44.50 g, 440 mmol) in ethanol (750 mL) was added ethyl 2-methyl-3-oxobutanoate (38.13 g, 264 mmol). The reaction was heated at 90° C. for 4 h. A further portion (6.36 g) of the ester was added and the reaction was stirred for 3 h. The reaction was concentrated to around 500 mL and stood overnight. Precipitation of the desired pyrimidinol (22.7 g) occurred. The mother liquors were concentrated and DCM and 1M HCl were added. The aqueous layer was extracted 7 times with DCM to give further crops of the desired product (total: 28.9 g, 56%) on concentration as a white solid.

Provenance & Evidence