Hydrochloric Acid → MS 857

Participants

Reaction Steps

In 40 ml of 50% aqueous solution of dimethylamine was dissolved 20 g of the 2-acetyl-4-(4-pyridyl)-cyclohexanone obtained by the above method (b) under ice cooling, and 30 g of acetoacetamide was added thereto. After stirring at room temperature for 2 days, the reaction mixture was neutralized with 6N hydrochloric acid under ice cooling. After allowed to stand for 1 hour under ice cooling, the resulting mixture was filtered to afford 12 g of crude crystals containing 3-4% of the above-said quinoline compound (IV) which was impurities. The crude crystals were recrystallized with 300 ml of methanol to afford 8 g of purified 4-acetyl-1-methyl-7-(4-pyridyl)-5,6,7,8-tetrahydro-3(2H)-isoquinolinone. The physical property values were as follows.

Provenance & Evidence