Formic Acid → HCID 23368487, compound

Participants

Reaction Steps

To 0.29 ml of formic acid is added 0.74 ml of acetic anhydride, and they are subjected to reaction at 40° C. for one hour. To the reaction mixture are added 5 ml of N,N-dimethylformamide and 1.00 g of 3-(2-amino-3-methoxypropoxy)-5-chloro-1,2-benzoisoxazole, and they are subjected to reaction at the same temperature for one hour. To the reaction mixture are added water and ethyl acetate, and after shaking, the organic layer is separated. Water is added again to the separated organic layer and the pH is adjusted to 8 with an aqueous sodium hydroxide solution, after which the organic layer is separated. The separated organic layer is washed with a saturated saline solution and dried over anhydrous magnesium sulfate, after which the solvent is removed by distillation under reduced pressure. Upon recrystallization from a mixed solvent of diisopropyl ether and ethyl acetate, there is obtained 0.50 g of colorless, crystalline 5-chloro-3-(2-formylamino-3-methoxypropoxy)-1,2-benzoisoxazole having a melting point of 90°-92° C.

Provenance & Evidence