Ethoxalyl chloride → HCID 44380397, compound

Participants

Reaction Conditions

Reaction Steps

With ice bath cooling, a solution of ethyl chlorooxoacetate (2.0 g, 14.6 mmol) in THF (25 ml) was dropwise added to a solution of 2-(3,4-dihydro-1H-isoquinolin-2-yl)-6-methyl-pyridin-4-yl-amine (example 4) (2.9 g, 12.1 mmol) in pyridine (40 ml). The mixture was stirred at 75° C. for 1 hr, evaporated and partitioned (AcOEt/NaHCO3-solution). The organic phase was dried (Na2SO4), concentrated and crystallized yielding 3.1 g (75%) of the title compound as light brown solid. Mp. 128-129° C. (AcOEt), MS: m/e=340 (M+H+).

Provenance & Evidence