Triethylamine → HCID 69026638, compound

Participants

Reaction Steps

0.3 g (1.17 mmol) of (+/−)10-amino-2-pyrimidin-4-yl-7,8,9,10-tetrahydropyrimido[1,2-a]azepin-4(6H)-one (compound 3.4 of example 3) was diluted in 8 mL of tetrahydrofuran. 0.18 mL (1.28 mmol) of triethylamine was added at 0° C. and the mixture was stirred for 10 min and 0.12 mL (1.28 mmol) of ethyl chloroformate was added. The resulting mixture was stirred at room temperature for 1 h and quenched by adding a saturated solution of ammonium chloride. The product was extracted with dichloromethane, dried over sodium sulfate and the solvent was evaporated. The residue was triturated with diethyl ether and filtered to afford 0.28 g (72%) of (4-oxo-2-pyrimidin-4-yl-4,6,7,8,9,10-hexahydro-pyrimido[1,2-a]azepin-10-yl)-carbamic acid ethyl ester as a yellow solid (Mp.: 168-170° C.). The compound was used as such in the next step.

Provenance & Evidence