Methyl acetoacetate → HCID 86757978, compound

Participants

Reaction Steps

444 g (6 mol) of calcium hydroxide was added to the kneader used in Comparative Example 1, and stirred. Thereafter, 1,532 g [13.2 mol, calcium hydroxide/methyl acetoacetate=1/2.2 (molar ratio)] of methyl acetoacetate was added dropwise to the kneader over 3 hours. The reaction temperature was between 36 and 58° C. After completion of the dropping, at a temperature of from 58 to 62° C., the reaction mixture was stirred and mixed for aging for 5 hours until the reaction was complete. The resulting product was warmed under a flow of nitrogen gas. When the temperature reached 62° C., the product was subjected to the drying step, and dried at 110 to 122° C. for 18 hours until the product attained a moisture content of 0.65% by weight. Thereafter, the dried product was cooled to give 1,618 g of white calcium methyl acetoacetate [yield 97.9 mol % (calcium hydroxide basis), purity 98.1% by weight].

Provenance & Evidence