We applied process analytical technologies to solve the problem of selectivity in the hydrogenation of 3-(2-chloroethyl)-9-hydroxy-2-methyl-4H-pyrido [1, 2-a] pyrimidin-4-one monohydrochloride (1) to (±) 3-(2-chloroethyl)-6, 7, 8, 9-tetrahydro-9-hydroxy-2-methyl-4H- pyrido [1, 2-a] pyrimidin-4-one monohydrochloride (2). We showed that both mid-IR and near-IR (NIR) were suitable for in-line analysis of the hydrogenation. We chose to use NIR ...