Sodium Methoxide → HCID 19745780, compound

Participants

Reaction Conditions

Reaction Steps

A solution of 1.08 g of sodium methylate in 10 ml of methanol is added at 20° C. while stirring to a solution of 7.65 g of 6-[2-chloro-6-oxo-4-trifluoromethyl-1(6H)pyrimidinyl]-4-(2-propynyl)-2H-1,4-benzoxazin-3(4H)-one in 300 ml of absolute methanol. A suspension forms during 15 minutes and the temperature rises to 30° C. The reaction mixture is concentrated at 40°-50° C. under reduced pressure and the residue is dissolved in 500 ml of ethyl acetate. The organic phase is washed twice with 200 ml of water each time, dried over anhydrous sodium sulphate and evaporated to dryness under reduced pressure. The crystalline residue is stirred with 20 ml of diethyl ether, cooled to 0° C. and treated with 100 ml of n-hexane. The crystals are filtered off under suction and dried at 50° C. under reduced pressure. In this manner there is obtained 6-[2-methoxy-6-oxo-4-trifluoromethyl-1(6H)-pyrimidinyl]-4-(2-propynyl)-2H-1,4-benzoxazin-3(4H)-one, m.p. 218°-220° C.

Provenance & Evidence