Acetone → HCID 131714215, compound

Participants

Reaction Conditions

Reaction Steps

16.1 g of 4 -hydroxyisocarbostyril was suspended in 160 ml of methanol, 21.1 g of 28% sodium methylate was added thereto to dissolve, and then 68.5 g of epibromohydrin was added and stirred for 1 hour at inner temperature of 60° C. The resulting reaction mixture was then concentrated under reduced pressure, and the residue obtained was extracted by adding water and chloroform. The chloroform layer thus obtained was washed with a saturated saline solution, dried over anhydrous sodium sulfate, then concentrated under reduced pressure. 11.8 g of the residue was dissolved in a mixed solvent of chloroform and methanol (19:1), purified over a column packed with 100 g of silica gel to obtain 5.0 g of the main fraction. The fraction was then dissolved in a mixed solvent of methanol and chloroform (1:1), then cooled after addition of acetone to separate a crystal. The crystal was taken out by filtration and then dried in vacuo to obtain 4.0 g of 4-(2,3-epoxy)propoxyisocarbostyril. m.p. 145°-149° C.

Provenance & Evidence