Diethyl Ether → 3-(2-Chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

Participants

Reaction Steps

At room temperature, 3-(2-chloroethyl)-2-methyl-9-benzyloxy-6,7,8,9-tetrahydro-pyrido[1,2-a]pyrimidin-4-one 4.0 g (0.0122 mole) was charged into a 250 mL three-necked bottle, 80 mL methanol was added, and then concentrated hydrochloric acid (about 25 drops) was added dropwise with stirring to adjust pH to 3.0. After the dissolution was completed, 1.8 g of wet 5% Pd—C (water content: 56%) (W/W: 10/1) was added, argon gas was fed to exchange atmosphere for three times, hydrogen gas was fed to exchange atmosphere for three times, the reaction was conducted at 27° C. for about 36 hours, and TLC (ethyl ether:n-hexane:methanol:triethylamine=2 mL:0.5 mL:6 drops:6 drops) was used to detect the debenzylated product. The reaction was stopped after all starting materials were consumed.

Provenance & Evidence