To produce a salt of ascorbyl-2-phosphate useful for a cosmetic or the like in a good efficiency, high purity and high yield by dissolving calcium ascorbate phosphate in an aqueous solution of ascorbyl phosphate within a prescribed acidic pH region, and treating the obtained solution under a specific condition.

Calcium ascorbate-2-phosphate of formula I (P is a group of formula II or the like) is dissolved in an aqueous solution of ascorbyl-2- phosphate of formula II (P1 is H2PO3, H3P2O6 or H4P3O9) at a pH value of 0.5-4, and calcium ion is removed from the obtained solution. The remaining solution is regulated so as to have 7-11 pH value by a sodium salt, a potassium salt, a magnesium salt or an aluminum salt, and the formula salt of ascorbyl-2- phosphate of formula IV [M is sodium, potassium, magnesium or aluminum; the product of (k).(m) is 3-5] is isolated to provide the objective salt of ascorbyl-2-phosphate of formula IV. The Ca++ is preferably removed by using an ion exchange resin of a strong acid.