Methyl acetoacetate → HCID 86757978, compound

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].

1. customwas between 36 and 58° C
2. stirringAfter completion of the dropping, at a temperature of from 58 to 62° C., the reaction mixture was stirred
3. additionmixed
4. temperatureThe resulting product was warmed under a flow of nitrogen gas
5. customreached 62° C.
6. customdried at 110 to 122° C. for 18 hours until the product
7. temperatureThereafter, the dried product was cooled

ORD record

ord-38aa66f7bb3a4a95b26bcb1d47b9a882

Source dataset

uspto-grants-2002_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06376719B1