HCID 18799436, compound → HCID 18799398, compound

Participants

Reaction Conditions

Reaction Steps

A solution of 3-[(3-chloro-2-chloromethyl-pyridin-4-yl)-methyl-amino]-propanol isolated in step a) (5.3 g) and 2-mercapto-benzimidazole (2.2 g, 14.6 mmol) in 2-propanol (150 ml) is boiled under reflux for 2 h. After cooling to 4° C. the precipitate is filtered, washed with 2-propanol and dried in vacua. The residue is dissolved in water, adjusted to pH 8 with aqueous sodium bicarbonate solution and extracted with ethyl acetate. The combined organic extracts are washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue is crystallized from ethyl acetate to give the title compound as an off-white solid, 3.6 g (46%). M.p. 127-30° C.

Provenance & Evidence